CN107021662B - 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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- CN107021662B CN107021662B CN201710337135.0A CN201710337135A CN107021662B CN 107021662 B CN107021662 B CN 107021662B CN 201710337135 A CN201710337135 A CN 201710337135A CN 107021662 B CN107021662 B CN 107021662B
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- cement
- grinding aid
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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
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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
- 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 fields of cement grinding, and in particular to a kind of preparation method of cement grinding aid.The present invention reacts itaconic acid with thionyl chloride to obtain acyl chlorides first, then acyl chlorides is reacted to obtain modified itaconic acid with the amino of glutamic 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, it prevents crackle from healing again and cement granules is inhibited to polymerize, there is the triethanolamine of grinding-aid effect to cement using lignin as the chemically modified access of raw material again, there is the very strong group of polarity in modified triethanolamine, strong surface-active is showed to prevent cement granules from coalescing, the effect stability of the resulting cement grinding aid of 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, It can store for a long time at different temperatures.
Description
Technical field
The invention belongs to the technical fields of cement grinding, and in particular to a kind of preparation method of cement grinding aid.
Background technique
Cement grinding is 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, improve the performance of grinding aid, it is that cement industry compels highly necessary to solve the problems, such as.
To reduce energy consumption, mill efficiency is improved, people are usually taken the measure in terms of following two: one, improve milling equipment and grinding
Technique to utilize mechanical energy to greatest extent；Two, cement grinding aid is added in cement pulverizing course and improves mill efficiency,
In second of measure be current field of cement production research emphasis.Cement grinding aid used at present has liquid grinding aid and consolidates
Body grinding aid, basis belong to greatly organic surface-active substance.
But there is also following deficiencies for effect of the cement grinding aid nowadays used in cement pulverizing course: (1) helping
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, especially
Existing on each age strength of cement influences, and significantly improve its intensity cannot；(3) to cement grinding energy consumption when improves not
Obviously, although moreover, current cement grinding aid can increase the addition content of mixing material, it will affect cement later strength.
And the cement grinding aid majority of function admirable is mixed by small organic molecule, the stability of this kind of grinding aid is poor,
Using effect fluctuation is larger, and applicable surface is relatively narrow.Therefore, a kind of effect stability, the good cement grinding aid tool of stability are researched and developed
There is important realistic meaning.
Summary of the invention
The technical problems to be solved by the invention: for the unstable defect of the effect of cement grinding aid used at present,
Provide a kind of preparation method of cement grinding aid.
In order to solve the above technical problems, the present invention uses technical solution as described below:
(1) after taking 30~40g itaconic acid and 200~300mL thionyl chloride to mix, at 60~120 DEG C back flow reaction 3~
4h obtains concentrate to which after reaction, product is concentrated；
(2) 50~60mL concentrate is taken to be added in three-necked flask, adding mass fraction is that 5% sodium hydroxide adjusts pH
After 7.2~7.5,15~20g glutamic acid is added, is stirred to react 1~2h at 75~85 DEG C, obtains modified itaconic acid mixing
Liquid；
(3) it weighs 1~2kg stalk to be crushed, be sieved, obtains stalk powder, 600~700g stalk powder is taken to carry out steam
Explosion, the material after obtaining explosion, by after explosion material and 1~2L mass fraction be 15% sodium hydroxide solution, 100~
It is filtered after 160 DEG C of 2~3h of immersion, obtains filter residue, i.e. lignin；
(4) after taking 35~40g lignin, 100~200mL water and the mixing of 6~8g triethanolamine, then 12~15mL ring is added dropwise
Oxygen chloropropane reacts 2~3h at 60~70 DEG C, filters after reaction, obtain filter cake, by Washing of Filter Cake, drying, ball milling,
Obtain powder；
(5) according to parts by weight, 15~20 parts of powder, 35~40 parts of modified itaconic acids, 5~8 parts of acrylic acid and 1~3 are taken
After part neopelex mixing, cement grinding aid is can be obtained in freeze-drying.
Preferably, the temperature of back flow reaction as described in step (1) is 60~70 DEG C.
Preferably, stalk described in step (3) is one or more of corn stover, wheat stalk, cotton stalk.
Preferably, the temperature of steam blasting described in step (3) is 220~230 DEG C, and pressure is 2.5~3.0MPa, is protected
The pressure time is 50~60s.
Preferably, the temperature of immersion described in step (3) is 150~160 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention flows back in thionyl chloride first using itaconic acid as raw material, obtains clothing health acyl chlorides, then by clothing health
The acid chloride groups of acyl chlorides react to obtain modified itaconic acid with the amino of glutamic acid, and modified itaconic acid is recycled to obtain with acroleic acid polymerization
To high molecular polymer, carboxyl and the adsorbable surface in cement granules of amide groups in high molecular polymer reduce cement
Surface can, prevent crackle from healing again and inhibit the polymerization of cement granules；
(2) present invention extracts from stalk again and obtains lignin, and then introducing lignin through chemical reaction has cement
The triethanolamine of grinding-aid effect contains polar group in modified lignin resin, shows strong surface-active to prevent cement
Grain coalescence, and triethanolamine can chelate the metal ion in cement, improve the early strength of cement, modified lignin resin and high score
Sub- polymer complex keeps grinding-aid effect more stable, while also improving the early strength of cement pair.
Specific embodiment
It weighs 30~40g itaconic acid to be added in the three-necked flask with thermometer and reflux unit, then adds into flask
Enter 200~300mL thionyl chloride, after being stirred 1~3min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus, in
Temperature is 60~70 DEG C, and revolving speed is 3~4h of back flow reaction under conditions of 260~300r/min；To the end of reacting, product is obtained,
Place the product in Rotary Evaporators, 30~40min of concentrated by rotary evaporation obtains concentrate, and 50~60mL concentrate is taken to be added to three
In mouth flask, then it is 7.2~7.5 that the pH that mass fraction is material in 5% sodium hydroxide solution adjusting flask, which is added, into flask,
And move into flask in water-bath, control bath temperature is 75~85 DEG C, then 15~20g glutamic acid is added into flask, heat preservation
It is stirred to react 1~2h, stops heating after reaction, modified itaconic acid mixed liquor is obtained, weighs 1~2kg stalk and be added to powder
It is crushed in broken machine, crosses 80~100 meshes, obtain stalk powder, 600~700g stalk powder is taken to be added in steam blasting machine,
Control explosion built-in temperature is 220~230 DEG C, pressure is 2.5~3.0MPa, and pressure release after 50~60s of pressure maintaining connects material penetrating
It receives in kettle, the material after obtaining explosion, it is that 15% sodium hydroxide is molten that the material after explosion, which is added to, and fills 1~2L mass fraction
In the beaker of liquid, beaker is moved into oil bath pan, control oil bath temperature is 150~160 DEG C, filters, obtains after 2~3h of immersion treatment
To filter residue, i.e. lignin, 35~40g lignin is taken to be added in the three-necked flask with thermometer and reflux unit, then to burning
100~200mL water and 6~8g triethanolamine are added in bottle, after being stirred 1~3min, flask is moved into water-bath, control
Bath temperature is 60~70 DEG C, then 12~15mL epoxychloropropane is added dropwise into flask, and control rate of addition is 1~3mL/min；
After being added dropwise, it is stirred to react 2~3h, after reaction by the material filtering in flask, filter cake is obtained, filter cake is washed with water
It is placed in baking oven for 3~5 times, is dry 1~2h at 95~105 DEG C in temperature, the material after drying is placed in ball in ball mill
15~20min is ground, powder is obtained, according to parts by weight, weighs 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 stirred 3~5min and are placed in freeze drier,
It is to freeze 15~20h at -35~-25 DEG C in temperature, cement grinding aid can be obtained.The stalk is corn stover, wheat
One or more of stalk, cotton stalk.
Example 1
It weighs 30g itaconic acid to be added in the three-necked flask with thermometer and reflux unit, then is added into flask
After being stirred 1min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus for 200mL thionyl chloride, in temperature be 60 DEG C,
Revolving speed is back flow reaction 3h under conditions of 260r/min；To the end of reacting, product is obtained, place the product in Rotary Evaporators,
Concentrated by rotary evaporation 30min, obtains concentrate, takes 50mL concentrate to be added in three-necked flask, then mass fraction is added into flask
The pH that material in flask is adjusted for 5% sodium hydroxide solution is 7.2, and flask is moved into water-bath, and control bath temperature is 75
DEG C, then 15g glutamic acid is added into flask, insulated and stirred reacts 1h, stops heating after reaction, and it is mixed to obtain modified itaconic acid
Liquid is closed, 1kg corn stover is weighed and is added in pulverizer and crush, 80 meshes is crossed, obtains stalk powder, 600g stalk powder is taken to add
Enter into steam blasting machine, control explosion built-in temperature is 220 DEG C, pressure 2.5MPa, and pressure release after pressure maintaining 50s sprays material
Enter to receive in kettle, the material after obtaining explosion, it is that 15% sodium hydroxide is molten that the material after explosion, which is added to, and fills 1L mass fraction
In the beaker of liquid, beaker is moved into oil bath pan, control oil bath temperature is 150 DEG C, it is filtered after immersion treatment 2h, obtains filter residue,
That is lignin takes 35g lignin to be added in the three-necked flask with thermometer and reflux unit, then is added into flask
After being stirred 1min, flask is moved into water-bath for 100mL water and 6g triethanolamine, and control bath temperature is 60 DEG C, then to
12mL epoxychloropropane is added dropwise in flask, control rate of addition is 1mL/min；After being added dropwise, it is stirred to react 2h, reaction knot
By the material filtering in flask after beam, filter cake is obtained, filter cake 3 times is washed with water and is placed in baking oven, is to be done at 95 DEG C in temperature
Material after drying is placed in ball milling 15min in ball mill, obtains powder by dry 1h, according to parts by weight, weigh 15 parts of powder,
35 parts of modified itaconic acids, 5 parts of acrylic acid and 1 part of neopelex are added in beaker, are stirred 3min and are placed on
In freeze drier, it is to freeze 15h at -35 DEG C in temperature, cement grinding aid can be obtained.
Example 2
It weighs 40g itaconic acid to be added in the three-necked flask with thermometer and reflux unit, then is added into flask
After being stirred 3min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus for 300mL thionyl chloride, in temperature be 70 DEG C,
Revolving speed is back flow reaction 4h under conditions of 300r/min；To the end of reacting, product is obtained, place the product in Rotary Evaporators,
Concentrated by rotary evaporation 40min, obtains concentrate, takes 60mL concentrate to be added in three-necked flask, then mass fraction is added into flask
The pH that material in flask is adjusted for 5% sodium hydroxide solution is 7.5, and flask is moved into water-bath, and control bath temperature is 85
DEG C, then 20g glutamic acid is added into flask, insulated and stirred reacts 2h, stops heating after reaction, and it is mixed to obtain modified itaconic acid
Liquid is closed, 2kg wheat stalk is weighed and is added in pulverizer and crush, sieves with 100 mesh sieve, obtains stalk powder, take 700g stalk powder
It is added in steam blasting machine, control explosion built-in temperature is 230 DEG C, pressure 3.0MPa, and pressure release after pressure maintaining 60s makes material
It sprays into and receives in kettle, the material after obtaining explosion, it is 15% sodium hydroxide that the material after explosion, which is added to, and fills 2L mass fraction
In the beaker of solution, beaker is moved into oil bath pan, control oil bath temperature is 160 DEG C, filters, is filtered after immersion treatment 3h
Slag, i.e. lignin take 40g lignin to be added in the three-necked flask with thermometer and reflux unit, then are added into flask
After being stirred 3min, flask is moved into water-bath for 200mL water and 8g triethanolamine, and control bath temperature is 70 DEG C, then to
15mL epoxychloropropane is added dropwise in flask, control rate of addition is 3mL/min；After being added dropwise, it is stirred to react 3h, reaction knot
By the material filtering in flask after beam, filter cake is obtained, filter cake 5 times is washed with water and is placed in baking oven, is to be done at 105 DEG C in temperature
Material after drying is placed in ball milling 20min in ball mill, obtains powder by dry 2h, according to parts by weight, weigh 20 parts of powder,
40 parts of modified itaconic acids, 8 parts of acrylic acid and 3 parts of neopelexes are added in beaker, are stirred 5min and are placed on
In freeze drier, it is to freeze 20h at -25 DEG C in temperature, cement grinding aid can be obtained.
Example 3
It weighs 35g itaconic acid to be added in the three-necked flask with thermometer and reflux unit, then is added into flask
After being stirred 2min, flask immigration digital display constant temperature is tested the speed in magnetic stirring apparatus for 250mL thionyl chloride, in temperature be 65 DEG C,
Revolving speed is back flow reaction 3.5h under conditions of 280r/min；To the end of reacting, product is obtained, place the product in Rotary Evaporators
In, concentrated by rotary evaporation 35min obtains concentrate, takes 55mL concentrate to be added in three-necked flask, then quality point is added into flask
Number is that the pH that 5% sodium hydroxide solution adjusts material in flask is 7.4, and flask is moved into water-bath, and control bath temperature is
80 DEG C, then 18g glutamic acid is added into flask, insulated and stirred reacts 1.5h, stops heating after reaction, obtains modified clothing health
Sour mixed liquor, weighs 1.5kg cotton stalk and is added in pulverizer and crush, and crosses 90 meshes, obtains stalk powder, take 650g stalk
Powder is added in steam blasting machine, and control explosion built-in temperature is 225 DEG C, pressure 2.8MPa, and pressure release after pressure maintaining 55s makes
Material, which sprays into, to be received in kettle, the material after obtaining explosion, and it is 15% hydrogen that the material after explosion, which is added to, and fills 1.5L mass fraction
In the beaker of sodium hydroxide solution, beaker is moved into oil bath pan, control oil bath temperature is 155 DEG C, it is filtered after immersion treatment 2.5h,
Filter residue, i.e. lignin are obtained, 38g lignin is taken to be added in the three-necked flask with thermometer and reflux unit, then to flask
After being stirred 2min, flask is moved into water-bath for middle addition 150mL water and 7g triethanolamine, and control bath temperature is 65
DEG C, then 17mL epoxychloropropane is added dropwise into flask, control rate of addition is 2mL/min；After being added dropwise, it is stirred to react
2.5h obtains filter cake after reaction by the material filtering in flask, is washed with water filter cake 4 times and is placed in baking oven, Yu Wendu
It is dry 1.5h at 100 DEG C, the material after drying is placed in ball milling 18min in ball mill, obtains powder, according to parts by weight,
It weighs 18 parts of powder, 38 parts of modified itaconic acids, 7 parts of acrylic acid and 2 parts of neopelexes to be added in beaker, stirring is mixed
It closes 4min to be placed in freeze drier, is to freeze 18h at -30 DEG C in temperature, cement grinding aid can be obtained.
The volume of the cement grinding aid 1:1000 in mass ratio prepared in present example 1~3 is subjected to cement grinding,
The performance for measuring cement is as shown in the table:
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of cement grinding aid, it is characterised in that specific preparation step are as follows:
(1) after taking 30~40g itaconic acid and 200~300mL thionyl chloride to mix, 3~4h of back flow reaction at 60~120 DEG C,
To which after reaction, product is concentrated, concentrate is obtained；
(2) 50~60mL concentrate is taken to be added in three-necked flask, add mass fraction be 5% sodium hydroxide adjust pH be 7.2
After~7.5,15~20g glutamic acid is added, is stirred to react 1~2h at 75~85 DEG C, obtains modified itaconic acid mixed liquor；
(3) it weighs 1~2kg stalk to be crushed, be sieved, obtains stalk powder, take 600~700g stalk powder to carry out steam quick-fried
It is broken, the material after obtaining explosion, by after explosion material and 1~2L mass fraction be 15% sodium hydroxide solution, 100~160
DEG C impregnate 2~3h after filter, obtain filter residue, i.e. lignin；
(4) after taking 35~40g lignin, 100~200mL water and the mixing of 6~8g triethanolamine, then 12~15mL epoxy chlorine is added dropwise
Propane reacts 2~3h at 60~70 DEG C, filters after reaction, obtain filter cake, Washing of Filter Cake, drying, ball milling obtain
Powder；
(5) according to parts by weight, 15~20 parts of powder, 35~40 parts of modified itaconic acids, 5~8 parts of acrylic acid and 1~3 part ten are taken
After the mixing of dialkyl benzene sulfonic acids sodium, cement grinding aid is can be obtained in freeze-drying.
2. a kind of preparation method of cement grinding aid according to claim 1, which is characterized in that as described in step (1)
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, which is characterized in that described in step (3)
Stalk is one or more of corn stover, wheat stalk, cotton stalk.
4. a kind of preparation method of cement grinding aid according to claim 1, which is characterized in that described in step (3)
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, which is characterized in that described in step (3)
The temperature of immersion is 150~160 DEG C.
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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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