CN107021662A - A kind of preparation method of cement grinding aid - Google Patents
A kind of preparation method of cement grinding aid Download PDFInfo
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- CN107021662A CN107021662A CN201710337135.0A CN201710337135A CN107021662A CN 107021662 A CN107021662 A CN 107021662A CN 201710337135 A CN201710337135 A CN 201710337135A CN 107021662 A CN107021662 A CN 107021662A
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- cement
- grinding aid
- cement grinding
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- 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)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the technical field of cement grinding, and in particular to a kind of preparation method of cement grinding aid.Itaconic acid and thionyl chloride reaction are obtained acyl chlorides by the present invention first, then the amino reaction of acyl chlorides and glutamic acid is obtained being modified itaconic acid, modified itaconic acid can generate stable type polymer with acroleic acid polymerization, carboxyl and amide groups in polymer it is adsorbable in cement particle surface and reduce the surface of cement can, prevent crackle heal and suppress again cement granules polymerize, again the triethanolamine for having grinding-aid effect to cement is accessed using lignin as raw material is chemically modified, there is polarity very strong group in modified triethanolamine, strong surface-active is showed to prevent cement granules from coalescing, the effect stability of cement grinding aid obtained by the present invention, improve the intensity of cement, compared with conventional cement grinding aid, 8~10Mpa is enhanced using the compression strength of cement after 1~2 day, and present invention gained cement grinding aid stability is good, can long-term storage at different temperatures.
Description
Technical field
The invention belongs to the technical field of cement grinding, and in particular to a kind of preparation method of cement grinding aid.
Background technology
Cement grinding, is the necessary process and key link in cement production process.Nowadays, people increasingly pay attention to low
Carbocyclic ring is protected, so energy-saving and emission-reduction, develop low-carbon economy, improves the performance of grinding aid, is the problem of cement industry compels highly necessary to solve.
For reduction power consumption, mill efficiency is improved, the measure of following two aspects is usually taken in people：One, improve milling equipment and grinding
Technique with to greatest extent utilize mechanical energy；Two, cement grinding aid is added in cement pulverizing course to improve mill efficiency, its
In second of measure be current field of cement production research emphasis.The cement grinding aid used at present has liquid grinding aid and solid
Body grinding aid, its basis belongs to greatly organic surface-active substance.
But, effect of the cement grinding aid nowadays used in cement pulverizing course also has the following disadvantages：（1）Help
Mill effect is unstable, and the cement fineness and specific surface area that grinding comes out need improve；（2）To the application performance of cement, particularly
There is influence to each age strength of cement, its intensity is significantly improved；（3）Energy consumption during to cement grinding improves not
Substantially, although moreover, current cement grinding aid can increase the addition content of mixing material, cement later strength can be influenceed.
And the cement grinding aid majority of function admirable is mixed by small organic molecule, the less stable of this kind of grinding aid,
Using effect fluctuation is larger, and applicable surface is narrower.Therefore, a kind of effect stability, the good cement grinding aid tool of stability are researched and developed
There is important realistic meaning.
The content of the invention
The technical problems to be solved by the invention：The unstable defect of the effect of cement grinding aid for using at present,
There is provided a kind of preparation method of cement grinding aid.
In order to solve the above technical problems, the present invention uses technical scheme as described below：
（1）Take after 30~40g itaconic acids and the mixing of 200~300mL thionyl chlorides, 3~4h of back flow reaction at 60~120 DEG C,
After question response terminates, product is concentrated, concentrate is obtained；
（2）50~60mL concentrates are taken to be added in three-necked flask, it is that 5% sodium hydroxide regulation pH is 7.2 to add mass fraction
After~7.5,15~20g glutamic acid is added, in 75~85 DEG C of 1~2h of stirring reaction, obtains being modified itaconic acid mixed liquor；
（3）Weigh 1~2kg stalks it is size-reduced, sieving, obtain stalk powder, take 600~700g stalk powders carry out steam it is quick-fried
It is broken, the material after explosion is obtained, is 15% sodium hydroxide solution by the material after explosion and 1~2L mass fractions, 100~160
DEG C immersion 2~3h after filter, obtain filter residue, i.e. lignin；
（4）Take after 35~40g lignin, 100~200mL water and the mixing of 6~8g triethanolamines, then 12~15mL epoxy chlorine is added dropwise
Propane, reacts 2~3h at 60~70 DEG C, and reaction is filtered after terminating, obtains filter cake, Washing of Filter Cake, drying, ball milling are obtained
Powder；
（5）Count by weight, take 15~20 parts of powder, 35~40 parts of modified itaconic acids, 5~8 parts of acrylic acid and 1~3 part ten
After the mixing of dialkyl benzene sulfonic acids sodium, freeze-drying, you can obtain cement grinding aid.
It is preferred that, step（1）Described in back flow reaction temperature be 60~70 DEG C.
It is preferred that, step（3）Described in stalk be maize straw, wheat stalk, cotton stalk in one or more.
It is preferred that, step（3）Described in steam blasting temperature be 220~230 DEG C, pressure be 2.5~3.0MPa, protect
The pressure time is 50~60s.
It is preferred that, step（3）Described in immersion temperature be 150~160 DEG C.
The present invention is compared with other method, and advantageous effects are：
（1）The present invention flows back first in thionyl chloride using itaconic acid as raw material, clothing health acyl chlorides is obtained, then by clothing health acyl chlorides
Acid chloride groups and the amino reaction of glutamic acid obtain being modified itaconic acid, recycle modified itaconic acid to obtain height with acroleic acid polymerization
The adsorbable surface in cement granules of carboxyl and amide groups in Molecularly Imprinted Polymer, high molecular polymer, reduces the surface of cement
Can, prevent crackle from healing and suppress again the polymerizations of cement granules；
（2）The present invention extracts from stalk and obtains lignin again, and then introduce lignin through chemical reaction has grinding aid to cement
Contain polar group in the triethanolamine of effect, modified lignin resin, show strong surface-active to prevent cement granules from gathering
Knot, and triethanolamine can chelate the metal ion in cement, improve the early strength of cement, modified lignin resin and polyphosphazene polymer
Compound, which coordinates, makes grinding-aid effect more stablize, while also improving the early strength of cement pair.
Embodiment
Weigh 30~40g itaconic acids to be added in the three-necked flask with thermometer and reflux, then add into flask
Enter 200~300mL thionyl chlorides, after 1~3min of stirring mixing, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus, in
Temperature is 60~70 DEG C, and rotating speed is 3~4h of back flow reaction under conditions of 260~300r/min；Question response terminates, and obtains product,
Product is placed in Rotary Evaporators, 30~40min of concentrated by rotary evaporation obtains concentrate, takes 50~60mL concentrates to be added to three
In mouth flask, then it is 7.2~7.5 to add the pH that mass fraction is material in 5% sodium hydroxide solution regulation flask into flask,
And move into flask in water-bath, it is 75~85 DEG C to control bath temperature, then adds 15~20g glutamic acid into flask, is incubated
1~2h of stirring reaction, reaction stops heating after terminating, and obtains being modified itaconic acid mixed liquor, weighs 1~2kg stalks and be added to powder
Crushed in broken machine, cross 80~100 mesh sieves, obtain stalk powder, take 600~700g stalk powders to be added in steam blasting machine,
Controlled blasting built-in temperature is 220~230 DEG C, pressure is pressure release after 2.5~3.0MPa, 50~60s of pressurize, sprays into material and connects
Receive in kettle, obtain the material after explosion, it is that 15% sodium hydroxide is molten that the material after explosion, which is added to, and fills 1~2L mass fractions
In the beaker of liquid, beaker is moved into oil bath pan, it is filtering after 150~160 DEG C, 2~3h of immersion treatment to control oil bath temperature, is obtained
To filter residue, i.e. lignin, 35~40g lignin is taken to be added in the three-necked flask with thermometer and reflux, then to burning
Add after 100~200mL water and 6~8g triethanolamines, 1~3min of stirring mixing, flask is moved into water-bath, control in bottle
Bath temperature is 60~70 DEG C, then 12~15mL epoxychloropropane is added dropwise into flask, and it is 1~3mL/min to control rate of addition；
After after completion of dropping, 2~3h of stirring reaction reacts the material filtering in flask after terminating, obtains filter cake, filter cake is washed with water
It is placed in after 3~5 times in baking oven, dries 1~2h at temperature is 95~105 DEG C, dried material is placed in ball in ball mill
Grind 15~20min, obtain powder, count by weight, weigh 15~20 parts of powder, 35~40 parts of modified itaconic acids, 5~8 parts
Acrylic acid and 1~3 part of neopelex are added in beaker, are placed in after 3~5min of stirring mixing in freeze drier,
15~20h is freezed at temperature is -35~-25 DEG C, you can obtain cement grinding aid.Described stalk is maize straw, wheat
One or more in stalk, cotton stalk.
Example 1
30g itaconic acids are weighed to be added in the three-necked flask with thermometer and reflux, then the addition 200mL chlorine into flask
Change after sulfoxide, stirring mixing 1min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus, is 60 DEG C in temperature, rotating speed is
Back flow reaction 3h under conditions of 260r/min；Question response terminates, and obtains product, and product is placed in Rotary Evaporators, rotates dense
Contracting 30min, obtains concentrate, takes 50mL concentrates to be added in three-necked flask, then it is 5% hydrogen to add mass fraction into flask
The pH of material is 7.2 in sodium hydroxide solution regulation flask, and flask is moved into water-bath, and it is 75 DEG C to control bath temperature, then
15g glutamic acid is added into flask, insulated and stirred reaction 1h, reaction stops heating after terminating, obtains being modified itaconic acid mixed liquor,
Weigh 1kg maize straws and be added to crushing in pulverizer, cross 80 mesh sieves, obtain stalk powder, take 600g stalk powders to be added to
In steam blasting machine, controlled blasting built-in temperature is 220 DEG C, pressure is pressure release after 2.5MPa, pressurize 50s, sprays into material and connects
Receive in kettle, obtain the material after explosion, it is 15% sodium hydroxide solution that the material after explosion, which is added to, and fills 1L mass fractions
In beaker, beaker is moved into oil bath pan, it is filtering after 150 DEG C, immersion treatment 2h to control oil bath temperature, obtains filter residue, i.e., wooden
Quality, takes 35g lignin to be added in the three-necked flask with thermometer and reflux, then the addition 100mL water into flask
With 6g triethanolamines, stirring is mixed after 1min, and flask is moved into water-bath, and it is 60 DEG C to control bath temperature, then into flask
12mL epoxychloropropane is added dropwise, it is 1mL/min to control rate of addition；After after completion of dropping, stirring reaction 2h, reaction will after terminating
Material filtering in flask, obtains filter cake, is placed in after filter cake 3 times is washed with water in baking oven, is to dry 1h at 95 DEG C in temperature, will
Dried material is placed in ball milling 15min in ball mill, obtains powder, counts by weight, weighs 15 parts of powder, 35 parts of modifications
Itaconic acid, 5 parts of acrylic acid and 1 part of neopelex are added in beaker, and freeze-drying is placed in after stirring mixing 3min
In machine, 15h is freezed at temperature is -35 DEG C, you can obtain cement grinding aid.
Example 2
40g itaconic acids are weighed to be added in the three-necked flask with thermometer and reflux, then the addition 300mL chlorine into flask
Change after sulfoxide, stirring mixing 3min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus, is 70 DEG C in temperature, rotating speed is
Back flow reaction 4h under conditions of 300r/min；Question response terminates, and obtains product, and product is placed in Rotary Evaporators, rotates dense
Contracting 40min, obtains concentrate, takes 60mL concentrates to be added in three-necked flask, then it is 5% hydrogen to add mass fraction into flask
The pH of material is 7.5 in sodium hydroxide solution regulation flask, and flask is moved into water-bath, and it is 85 DEG C to control bath temperature, then
20g glutamic acid is added into flask, insulated and stirred reaction 2h, reaction stops heating after terminating, obtains being modified itaconic acid mixed liquor,
Weigh 2kg wheat stalks and be added to crushing in pulverizer, cross 100 mesh sieves, obtain stalk powder, take 700g stalk powders to be added to
In steam blasting machine, controlled blasting built-in temperature is 230 DEG C, pressure is pressure release after 3.0MPa, pressurize 60s, sprays into material and connects
Receive in kettle, obtain the material after explosion, it is 15% sodium hydroxide solution that the material after explosion, which is added to, and fills 2L mass fractions
In beaker, beaker is moved into oil bath pan, it is filtering after 160 DEG C, immersion treatment 3h to control oil bath temperature, obtains filter residue, i.e., wooden
Quality, takes 40g lignin to be added in the three-necked flask with thermometer and reflux, then the addition 200mL water into flask
With 8g triethanolamines, stirring is mixed after 3min, and flask is moved into water-bath, and it is 70 DEG C to control bath temperature, then into flask
15mL epoxychloropropane is added dropwise, it is 3mL/min to control rate of addition；After after completion of dropping, stirring reaction 3h, reaction will after terminating
Material filtering in flask, obtains filter cake, is placed in after filter cake 5 times is washed with water in baking oven, is to dry 2h at 105 DEG C in temperature,
Dried material is placed in ball milling 20min in ball mill, powder is obtained, counts by weight, weigh 20 parts of powder, 40 parts change
Property itaconic acid, 8 parts of acrylic acid and 3 parts of neopelexes be added in beaker, it is dry to be placed in freezing after stirring mixing 5min
In dry machine, 20h is freezed at temperature is -25 DEG C, you can obtain cement grinding aid.
Example 3
35g itaconic acids are weighed to be added in the three-necked flask with thermometer and reflux, then the addition 250mL chlorine into flask
Change after sulfoxide, stirring mixing 2min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus, is 65 DEG C in temperature, rotating speed is
Back flow reaction 3.5h under conditions of 280r/min；Question response terminates, and obtains product, and product is placed in Rotary Evaporators, revolving
35min is concentrated, concentrate is obtained, takes 55mL concentrates to be added in three-necked flask, then it is 5% to add mass fraction into flask
The pH of material is 7.4 in sodium hydroxide solution regulation flask, and flask is moved into water-bath, and it is 80 DEG C to control bath temperature,
18g glutamic acid is added into flask again, insulated and stirred reaction 1.5h, reaction stops heating after terminating, obtains being modified itaconic acid and mix
Liquid is closed, 1.5kg cotton stalks is weighed and is added to crushing in pulverizer, cross 90 mesh sieves, obtain stalk powder, take 650g stalk powders
It is added in steam blasting machine, controlled blasting built-in temperature is 225 DEG C, pressure is pressure release after 2.8MPa, pressurize 55s, makes material
Spray into and receive in kettle, obtain the material after explosion, the material after explosion is added to and fills 1.5L mass fractions for 15% hydroxide
In the beaker of sodium solution, beaker is moved into oil bath pan, it is filtering after 155 DEG C, immersion treatment 2.5h to control oil bath temperature, is obtained
Filter residue, i.e. lignin, take 38g lignin to be added in the three-necked flask with thermometer and reflux, then add into flask
Enter after 150mL water and 7g triethanolamines, stirring mixing 2min, flask is moved into water-bath, it is 65 DEG C to control bath temperature, then
17mL epoxychloropropane is added dropwise into flask, it is 2mL/min to control rate of addition；After after completion of dropping, stirring reaction 2.5h, instead
By the material filtering in flask after should terminating, obtain filter cake, be placed in after filter cake 4 times is washed with water in baking oven, in temperature be 100 DEG C
Lower dry 1.5h, ball milling 18min in ball mill is placed in by dried material, is obtained powder, is counted by weight, weighs 18 parts
Powder, 38 parts of modified itaconic acids, 7 parts of acrylic acid and 2 parts of neopelexes are added in beaker, after stirring mixing 4min
It is placed in freeze drier, freezes 18h at temperature is -30 DEG C, you can obtain cement grinding aid.
By the cement grinding aid in mass ratio 1 prepared in present example 1~3:1000 volume carries out cement grinding,
The performance for measuring cement is as shown in the table：
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by above-described embodiment
System, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of cement grinding aid, it is characterised in that specifically preparation process is：
（1）Take after 30~40g itaconic acids and the mixing of 200~300mL thionyl chlorides, 3~4h of back flow reaction at 60~120 DEG C,
After question response terminates, product is concentrated, concentrate is obtained；
（2）50~60mL concentrates are taken to be added in three-necked flask, it is that 5% sodium hydroxide regulation pH is 7.2 to add mass fraction
After~7.5,15~20g glutamic acid is added, in 75~85 DEG C of 1~2h of stirring reaction, obtains being modified itaconic acid mixed liquor；
（3）Weigh 1~2kg stalks it is size-reduced, sieving, obtain stalk powder, take 600~700g stalk powders carry out steam it is quick-fried
It is broken, the material after explosion is obtained, is 15% sodium hydroxide solution by the material after explosion and 1~2L mass fractions, 100~160
DEG C immersion 2~3h after filter, obtain filter residue, i.e. lignin；
（4）Take after 35~40g lignin, 100~200mL water and the mixing of 6~8g triethanolamines, then 12~15mL epoxy chlorine is added dropwise
Propane, reacts 2~3h at 60~70 DEG C, and reaction is filtered after terminating, obtains filter cake, Washing of Filter Cake, drying, ball milling are obtained
Powder；
（5）Count by weight, take 15~20 parts of powder, 35~40 parts of modified itaconic acids, 5~8 parts of acrylic acid and 1~3 part ten
After the mixing of dialkyl benzene sulfonic acids sodium, freeze-drying, you can obtain cement grinding aid.
2. a kind of preparation method of cement grinding aid according to claim 1, it is characterised in that step（1）Described in
The temperature of back flow reaction is 60~70 DEG C.
3. a kind of preparation method of cement grinding aid according to claim 1, it is characterised in that step（3）Described in
Stalk is the one or more in maize straw, wheat stalk, cotton stalk.
4. a kind of preparation method of cement grinding aid according to claim 1, it is characterised in that step（3）Described in
The temperature of steam blasting is 220~230 DEG C, and pressure is 2.5~3.0MPa, and the dwell time is 50~60s.
5. a kind of preparation method of cement grinding aid according to claim 1, it is characterised in that step（3）Described in
The temperature of immersion is 150~160 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271876A (en) * | 2015-10-20 | 2016-01-27 | 章丘华明水泥有限公司 | Cement grinding aid |
| CN105693132A (en) * | 2016-01-28 | 2016-06-22 | 桂林华越环保科技有限公司 | Preparation method of special grinding aid for silver grey rock powder |
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2017
- 2017-05-14 CN CN201710337135.0A patent/CN107021662B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271876A (en) * | 2015-10-20 | 2016-01-27 | 章丘华明水泥有限公司 | Cement grinding aid |
| CN105693132A (en) * | 2016-01-28 | 2016-06-22 | 桂林华越环保科技有限公司 | Preparation method of special grinding aid for silver grey rock powder |
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Effective date of registration: 20190312 Address after: 233111 Liufu Town, Fengyang County, Chuzhou City, Anhui Province Applicant after: Fengyang Zhongdu Cement Co., Ltd. Address before: 213102 No. 35, 99-4 Huangshan Road, Xinbei District, Changzhou City, Jiangsu Province Applicant before: Changzhou five glory Chemical Co., Ltd. |
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