CN106746845B - A kind of production technology of cement grinding aid - Google Patents
A kind of production technology of cement grinding aid Download PDFInfo
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- CN106746845B CN106746845B CN201611030530.6A CN201611030530A CN106746845B CN 106746845 B CN106746845 B CN 106746845B CN 201611030530 A CN201611030530 A CN 201611030530A CN 106746845 B CN106746845 B CN 106746845B
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- reaction
- grinding aid
- production technology
- cement grinding
- ethylene oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
- C04B24/122—Hydroxy amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/52—Grinding aids; Additives added during grinding
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of production technologies of cement grinding aid, its key points of the technical solution are that including following preparation process：Step 1：Reaction kettle forevacuum, negative pressure sucking diethanol amine and water, open the circulation pump make Matter Transfer；Step 2：It is passed through nitrogen displacement, is replaced altogether three times；Step 3：Propylene oxide is added after heat temperature raising, carries out addition reaction；Step 4：Ethylene oxide is added after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is automatically closed, and material continues cycling through, and waits for that ethylene oxide fully reacts, reaction terminates.It can all be increased in early strength and later strength by cement adjuvant made from above-mentioned reaction step.
Description
Technical field
The present invention relates to cement grinding aid field, more particularly to a kind of production technology of cement grinding aid.
Background technology
Most of energy consumption is consumed in cement pulverizing course in cement industry, and the capacity usage ratio pole of cement grinding
Low, 95% energy loses as thermal energy.
Currently, during cement is milled, cement grinding aid, which is added, can reduce the grinding time of clinker, can drop
Cement particle surface free charge density in low grinding process reduces the free energy of the surface of solids, is mutually touched between reduction particle
It hits, prevents particle from the probability adhered to of reuniting occurs, reduce cement cost and the intensity of cement can be effectively improved.
Diethanol monoisopropanolamine is mainly applied in cement grinding aid at present, and volume is ten thousand/zero of cement quality
2/50000 to ten thousand, it can both can be designed as high additive with polyalcohol, triethanolamine and harmless inorganic salts Application of composite
Product is for high-mark cement to reach the resultant effect that enhancing proposes production.
Application No. is the Chinese patents of 200810124206.X to disclose a kind of continuous side for preparing high-efficiency concrete grinding aid
Method is that successive reaction is sent into ammonia logistics and propene oxide stream using ammonia, propylene oxide and ethylene oxide as raw material in the invention
Device is formed continuously the mixture containing monoisopropanolamine, diisopropanolamine (DIPA), triisopropanolamine, and the liquid level in flow reactor is made to protect
It holds and is being enough to make wherein logistics to carry out outer circulation spray through circulating pump from flow reactor bottom to top, while by fraction of stream
It is continuously introduced into the unreacted ammonia of removing in flash column；Then removing ammonia logistics is reacted with ethylene oxide stream, continuous
To product.But a large amount of side reaction can occur in the production process, the presence of side reaction product influences whether cement
Agent is applied in cement.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of production technology of cement grinding aid,
The early strength of cement and later strength is enabled to all to be improved in the application by the cement grinding aid of the technique productions.
The present invention above-mentioned technical purpose technical scheme is that：A kind of production of cement grinding aid
Technique, including following preparation process：
Step 1：Reaction kettle forevacuum, negative pressure sucking diethanol amine and water, open the circulation pump make Matter Transfer；
Step 2：It is passed through nitrogen displacement, is replaced altogether three times；
Step 3：Heating is slowly added to propylene oxide cycle, carries out addition reaction after heating；
Step 4：Ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is automatically closed,
Material continues cycling through, and waits for that ethylene oxide fully reacts, reaction terminates.
Through the above technical solutions, generating diethanol list isopropyl using diethanol amine and cyclopropane reaction in present specification
Hydramine, and the complete diethanol amine of unreacted can react with cyclohexane and generate triethanolamine, then the component generated includes two
The compounding ingredients of ethyl alcohol monoisopropanolamine and triethanolamine, diethanol monoisopropanolamine and triisopropanolamine and triethanolamine phase
Than, there is similar or equal basic characteristic dispersibility, but its comprehensive performance has apparent advantage, under similarity condition,
Early strength is higher than or is not less than triethanolamine, and later strength is far above triethanolamine；Early strength is far above three isopropanols
Amine, later strength are less than triisopropanolamine；Since diethanol monoisopropanolamine early strength is higher than or is not less than triethanolamine,
So the triethanolamine contained in component makes early strength also can further improve, and later strength also has guarantor simultaneously
Barrier；Simultaneously in process, it since diethanol amine is harmful substance, when sucking diethanol amine steam or mist, can pierce
Swash respiratory tract, so the mode for taking negative pressure to suck in this experiment, can avoid staff from directing contact with, nor
It will appear leakage, the influence caused by human body can be reduced；Being passed through nitrogen displacement in step 2 can be by the air in reaction kettle
Discharge, and due in replacement process material recycling, do not eliminated so still having some gases, thus nitrogen displacement carry out three
It is secondary；Propylene oxide is added after increasing in heating temperature after nitrogen replacement completion, since temperature is sufficiently high, so the reaction can be rapid
It carries out, reaction rate is very fast；It waits for addition after reaction, continuously adds ethylene oxide, ethylene oxide can be with unreacted diethyl
Hydramine reaction generates triethanolamine, and the raw material of reaction is fairly simple, and processing technology is also fairly simple, and the product generated is two
The combination product of kind compound, has good prospect of the application.
The present invention is further arranged to：Diethanol amine, propylene oxide and the ethylene oxide being added in the production technology
Molar ratio is 1:0.87~0.97:0.03~0.13.
Through the above technical solutions, the molar ratio of the diethanol amine, propylene oxide and ethylene oxide in component is above-mentioned
Ratio range, the purity of the product of the diethanol monoisopropanolamine generated by the reaction system of experimental verification in the range
Relatively high, high boiling point by-products produced content therein also can be relatively low, to can all have in terms of the purity and appearance of product higher
Quality, and the addition of ethylene oxide can also promote reaction carry out so that react progress more thoroughly.
The present invention is further arranged to：It is heated using steam in step 3.
Through the above technical solutions, being heated using steam, heating speed is fast, and the thermal efficiency is high, so as to save it is economical at
This.
The present invention is further arranged to：Temperature in step 3 is heated to 55~60 DEG C.
Through the above technical solutions, propylene oxide is added after being heated to 55~60 degree in temperature, temperature is controlled in the range
Interior one side is, so increasing temperature can avoid crystallizing, to promote reaction since diethanol amine can form crystallization at normal temperatures
It is smoothed out.
The present invention is further arranged to：Addition reaction in step 3 generates heat and is spread out of by heat exchanger system.
Through the above technical solutions, due to meeting reaction of formation heat in the third reaction process of diethanol amine and epoxy, cause to react
Temperature in kettle increases, and temperature raising can make reaction that side reaction occur to generate by-product, and the presence of by-product can influence
Influence to grinding aid to the intensity of cement, and reaction heat discharge can then be inhibited to the generation of side reaction.
The present invention is further arranged to：Temperature in step 3 is heated to 63~67 DEG C.
Through the above technical solutions, reaction temperature control is in the range, the rate of reaction is enabled to be maintained at one
Side reaction in the range of faster, and within this temperature range can be smaller, and the high boiling by-product generated contains
Amount also will be corresponding relatively low, then the by-product that the diethanol monoisopropanolamine generated contains will be relatively low, then is applying
Influence of the byproduct in process object to using effect also will be smaller.
The present invention is further arranged to：Step 3 addition reaction carries out 3h.
Through the above technical solutions, by lot of experiment validation, reaction time control enables to reaction to carry out in 3h
More completely, the yield of the product of generation is higher.
The present invention is further arranged to：Pressure in the reaction kettle is 0.2MPa.
Through the above technical solutions, the pressure control in reaction kettle enables to the rate of reaction to be maintained at one in 0.2MPa
In a higher range, accelerate reaction rate.
The present invention is further arranged to：The Matter Transfer time in step 4 is set as 20~25min.
Through the above technical solutions, reaction time control can be realized in the range than more completely reacting, can keep away
The waste of raw material caused by exempting from time too short caused reaction not exclusively, while can also avoid the reaction time long caused
By-product it is excessive.
In conclusion the present invention having the beneficial effect that in contrast to the prior art：
1, the proportioning in reacting between each raw material is maintained in reasonable range, the product diethanol monoisopropanolamine generated
With the mixture of triethanolamine, in application, it is all improved in early strength and later stage in cement, compared to simple two
Ethyl alcohol monoisopropanolamine its have apparent humidification in performance；
2, addition propylene oxide and ethylene oxide are added using substep in component, are enabled to the more thorough of reaction, are carried
The production rate of high primary product；
3, reaction time and temperature control are reasonable, can effectively reduce the generation of by-product, influence the service efficiency of product.
Specific implementation mode
Invention is further described in detail with reference to embodiments.
A kind of production technology of cement grinding aid
Embodiment 1
Step 1：Reaction kettle forevacuum, negative pressure sucking 500Kg diethanol amine and 105Kg water, open the circulation pump make material send out
Raw cycle；
Step 2：It is passed through nitrogen displacement three times, the air in reaction kettle is discharged；
Step 3：Temperature is heated to be slowly added to the progress addition reaction of 240.3Kg propylene oxide, addition reaction after 55 DEG C
Temperature control be 63 DEG C, pressure 0.2MPa, reaction generate heat is spread out of with controlling reaction temperature by heat exchanger system, react into
Row 3h；Step 4：27.2Kg ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve closes automatically
It closes, material continues cycling through reaction 20min, waits for that ethylene oxide fully reacts, reaction terminates.
Embodiment 2
Step 1：Reaction kettle forevacuum, negative pressure sucking 500Kg diethanol amine and 105Kg water, open the circulation pump make material send out
Raw cycle；
Step 2：It is passed through nitrogen displacement three times, the air in reaction kettle is discharged；
Step 3：Temperature is heated to be slowly added to the progress addition reaction of 245.8Kg propylene oxide, addition reaction after 56 DEG C
Temperature control is 64 DEG C, pressure 0.2MPa, and reaction generates heat and spread out of with controlling reaction temperature by heat exchanger system；
Step 4：23.0Kg ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is certainly
Dynamic to close, material continues cycling through reaction 21min, waits for that ethylene oxide fully reacts, reaction terminates.
Embodiment 3
Step 1：Reaction kettle forevacuum, negative pressure sucking 500Kg diethanol amine and 105Kg water, open the circulation pump make material send out
Raw cycle；
Step 2：It is passed through nitrogen displacement three times, the air in reaction kettle is discharged；
Step 3：Temperature is heated to be slowly added to the progress addition reaction of 251.3Kg propylene oxide, addition reaction after 57 DEG C
Temperature control is 65 DEG C, pressure 0.2MPa, and reaction generates heat and spread out of with controlling reaction temperature by heat exchanger system；
Step 4：18.9Kg ethylene oxide is added after terminating slowly in addition reaction, and the reaction was continued, and charging terminates, and inlet valve is certainly
Dynamic to close, material continues cycling through reaction 22min, waits for that ethylene oxide fully reacts, reaction terminates.
Embodiment 4
Step 1：Reaction kettle forevacuum, negative pressure sucking 500Kg diethanol amine and 105Kg water, open the circulation pump make material send out
Raw cycle；
Step 2：It is passed through nitrogen displacement three times, the air in reaction kettle is discharged；
Step 3：Temperature is heated to be slowly added to the progress addition reaction of 256.9Kg propylene oxide, addition reaction after 58 DEG C
Temperature control is 66 DEG C, pressure 0.2MPa, and reaction generates heat and spread out of with controlling reaction temperature by heat exchanger system；
Step 4：14.7Kg ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is certainly
Dynamic to close, material continues cycling through reaction 23min, waits for that ethylene oxide fully reacts, reaction terminates.
Embodiment 5
Step 1：Reaction kettle forevacuum, negative pressure sucking 500Kg diethanol amine and 105Kg water, open the circulation pump make material send out
Raw cycle；
Step 2：It is passed through nitrogen displacement three times, the air in reaction kettle is discharged；
Step 3：Temperature is heated to be slowly added to the progress addition reaction of 262.4Kg propylene oxide, addition reaction after 59 DEG C
Temperature control is 67 DEG C, pressure 0.2MPa, and reaction generates heat and spread out of with controlling reaction temperature by heat exchanger system；
Step 4：8.4Kg ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is automatic
It closes, material continues cycling through reaction 24min, waits for that ethylene oxide fully reacts, reaction terminates.
Embodiment 6
Step 1：Reaction kettle forevacuum, negative pressure sucking 500Kg diethanol amine and 105Kg water, open the circulation pump make material send out
Raw cycle；
Step 2：It is passed through nitrogen displacement three times, the air in reaction kettle is discharged；
Step 3：Temperature is heated to be slowly added to the progress addition reaction of 267.9Kg propylene oxide, addition reaction after 60 DEG C
Temperature control is 67 DEG C, pressure 0.2MPa, and reaction generates heat and spread out of with controlling reaction temperature by heat exchanger system；
Step 4：6.3Kg ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is automatic
It closes, material continues cycling through reaction 25min, waits for that ethylene oxide fully reacts, reaction terminates.
Experiment detection
1, grinding is tested
The small mill experimental study of grinding aid, cement material proportioning selection
| Clinker | Slag | Gypsum |
| 60% | 35% | 5% |
Material enters before mill through jaw crushing crusher machine, and material is added in the grinding aid in embodiment 1-6 in a manner of aqueous solution
In, it is poured into mill after uniform, grinding time 25min.
Analysis test method,
The square hole screen for tailing over measurement 0.08mm carries out dry screen by KGB45-77 methods；Blain specific surface, which measures, to be used
DBT-127 types Bo Shi breathes freely ratio surface area instrument, is carried out by KGB07-63 methods；
Particle size distribution uses KF-9 type Laser particle-size distribution analyzers, is as a result exported by computer；
Cement mortar strength test is according to KGB/T17671-1999.
The laboratory test results of 1 embodiment 1-6 of table
| Project | Tail over/% | Specific surface area m2/kKg | Average grain diameter/um | 28d compression strength/MPa | 28d flexural strengths/MPa |
| Embodiment 1 | 2.6 | 378 | 19 | 53.12 | 7.4 |
| Embodiment 2 | 2.4 | 376 | 19 | 53.21 | 7.41 |
| Embodiment 3 | 2.3 | 375 | 18 | 53.25 | 7.44 |
| Embodiment 4 | 2.25 | 380 | 17 | 53.41 | 7.5 |
| Embodiment 5 | 2.2 | 379 | 17 | 53.39 | 7.49 |
| Embodiment 6 | 2.1 | 380 | 16.5 | 53.40 | 7.48 |
By above table can with obtain, the properties in embodiment 1-6 meet the requirements of the standard, or even want excellent
In the range of prescribed by standard, by the way that the grinding aid of embodiment 1-6 is added in cement, and its properties is measured, pass through ratio
Compared with the experimental result in table, then it can be found that the using effect of the cement grinding aid of embodiment 4 is the most excellent, when the water of addition
When the amount of cement grinding aids gradually increases, using effect enhancing is not obvious.It is advantageous to embodiments 4 to be used as present specification
Optimum embodiment.
Comparative example 1
For comparative example 1 with embodiment difference lies in ethylene oxide is not added in comparative example 1, other keep one with embodiment
It causes.
Comparative example 2
Comparative example 2 is added to after being mixed with ethylene oxide difference lies in 2 oxypropylene of comparative example with embodiment reacts
In kettle, other are consistent with embodiment.
Comparative example 3
Grinding aid grinding is added without in cement material.
The laboratory test results of 2 comparative example 1-3 of table
| Project | Tail over/% | Specific surface area m2/kKg | Average grain diameter | 28d compression strength/MPa | 28d flexural strengths/MPa |
| Comparative example 1 | 2.6 | 371 | 25 | 51 | 7.20 |
| Comparative example 2 | 2.5 | 370 | 25 | 51.4 | 7.3 |
| Comparative example 3 | 2.8 | 360 | 58 | 49.8 | 7.1 |
| Embodiment 4 | 2.25 | 380 | 17 | 53.41 | 7.5 |
By the laboratory test results of comparative example 4 and comparative example 1, can significantly be obtained by the data in table
The properties of embodiment 4 are superior to comparative example 1, since difference lies in the cement in comparative example 1 with embodiment 4 for comparative example 1
Cyclohexane is not added in process for grinding aid, and other conditions do not change, so not contained in the component in comparative example 1
Triethanolamine, so the performance of product is declined；Continue to compare comparative example 2 and embodiment 4, the ring in comparative example 2
Ethane and cyclopropane are added simultaneously, and other conditions do not change, so can obtain comparative example 2 by contrast and experiment
Difference of the properties than embodiment 4, it is possible to reason out and propylene oxide and ethylene oxide are added separately in reaction kettle
Using effect to be substantially better than the effect being added at one time in reaction kettle；Comparative example 3 and embodiment 4 are compared, in comparative example 3
Cement in cement grinding aid is not added, then can show that cement grinding aid is not added makes cement by comparative test result
Milling performance is affected, so cement grinding aid, which is added, can largely change the performance of cement.
The above is only the exemplary embodiment of the present invention, protection domain and is not intended to limit the present invention, this hair
Bright protection domain is determined by the attached claims.
Claims (9)
1. a kind of production technology of cement grinding aid, it is characterized in that：Including following preparation process：
Step 1：Reaction kettle forevacuum, negative pressure sucking diethanol amine and water, open the circulation pump make Matter Transfer；
Step 2：It is passed through nitrogen displacement, is replaced altogether three times；
Step 3：Heating is slowly added to propylene oxide cycle, carries out addition reaction after heating；
Step 4：Ethylene oxide is slowly added to after addition reaction, and the reaction was continued, and charging terminates, and inlet valve is automatically closed, material
It continues cycling through, waits for that ethylene oxide fully reacts, reaction terminates.
2. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：It is added in the production technology
Diethanol amine, propylene oxide and ethylene oxide molar ratio be 1:0.87~0.97:0.03~0.13.
3. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：Added using steam in step 3
Heat.
4. a kind of production technology of cement grinding aid according to claim 3, it is characterized in that：Heating described in step 3
For temperature is heated to 55 ~ 60 DEG C.
5. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：Addition reaction in step 3
Heat is generated to spread out of by heat exchanger system.
6. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：The temperature of step 3 addition reaction
Degree control is at 63 ~ 67 DEG C.
7. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：Step 3 addition reaction carries out
3h。
8. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：Pressure in the reaction kettle
For 0.2MPa.
9. a kind of production technology of cement grinding aid according to claim 1, it is characterized in that：Matter Transfer in step 4
Time is set as 20 ~ 25min.
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| CN201611030530.6A CN106746845B (en) | 2016-11-16 | 2016-11-16 | A kind of production technology of cement grinding aid |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB704226A (en) * | 1952-03-24 | 1954-02-17 | Dow Chemical Co | Process for making polyalkanolamines |
| CN103204779A (en) * | 2013-04-27 | 2013-07-17 | 弗克科技(苏州)有限公司 | Alkylol amine and preparation method |
| CN103224453A (en) * | 2013-03-28 | 2013-07-31 | 宁波市联凯化学有限公司 | Method for preparing diethanol isopropanol amine |
| CN103936321A (en) * | 2013-01-17 | 2014-07-23 | 张恩源 | Composite early strength output increasing type grinding aid and preparation method thereof |
| CN103936602A (en) * | 2014-04-02 | 2014-07-23 | 四川鑫统领建材科技有限公司 | Method for joint production of isopropanolamine |
-
2016
- 2016-11-16 CN CN201611030530.6A patent/CN106746845B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB704226A (en) * | 1952-03-24 | 1954-02-17 | Dow Chemical Co | Process for making polyalkanolamines |
| CN103936321A (en) * | 2013-01-17 | 2014-07-23 | 张恩源 | Composite early strength output increasing type grinding aid and preparation method thereof |
| CN103224453A (en) * | 2013-03-28 | 2013-07-31 | 宁波市联凯化学有限公司 | Method for preparing diethanol isopropanol amine |
| CN103204779A (en) * | 2013-04-27 | 2013-07-17 | 弗克科技(苏州)有限公司 | Alkylol amine and preparation method |
| CN103936602A (en) * | 2014-04-02 | 2014-07-23 | 四川鑫统领建材科技有限公司 | Method for joint production of isopropanolamine |
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