CN105271912B - A kind of preparation method of starch base hydration heat of cement controlled material - Google Patents
A kind of preparation method of starch base hydration heat of cement controlled material Download PDFInfo
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- CN105271912B CN105271912B CN201510724386.5A CN201510724386A CN105271912B CN 105271912 B CN105271912 B CN 105271912B CN 201510724386 A CN201510724386 A CN 201510724386A CN 105271912 B CN105271912 B CN 105271912B
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Abstract
It is well mixed the invention provides a kind of preparation method of starch base hydration heat of cement controlled material, including by dextrin, starch and mixed dibasic acid acid anhydride in high-speed stirring mixer；By the mixture through double screw extruder melting extrusion, crush, screening produces product starch base hydration heat of cement controlled material.This method technique is simply efficient, and the reaction time is greatly shortened, while avoiding the use of solvent in preparation process, reduces harm of the discarded object to environment；The rate of heat release of aquation accelerated period and deceleration period can be greatly reduced in heat of hydration controlled material prepared by this method, and can effectively reduce hydration heat speed peak value more than 80%, significantly delay aquation induction period different from conventional set retarder.
Description
Technical field
The invention belongs to construction material concrete admixture field, and in particular to a kind of starch base hydration heat of cement regulates and controls material
The preparation method of material.
Background technology
The hydration reaction of cement is an exothermic reaction, and the concrete that cement plus water and other aggregate mixs are made is being poured
In rear condensation, hardening process, the substantial amounts of heat of hydration can be produced.Because concrete is the non-conductor of heat, and volume is larger, because
This heat of hydration is gathered in inside concrete and is difficult diverging, steeply rises internal temperature.Simultaneously as concrete surface radiating compared with
It hurry up, generate larger internal-external temperature difference, cause inside and outside thermal expansion and contraction degree different, and then tension is produced in concrete surface.
When tension exceedes concrete ultimate tensile strength, thermal cracking will be produced, this crack majority occurs in pouring
Later stage, intensity and durability to concrete produce harmful effect.In order to slow down concentration heat release of the concrete at the initial stage that pours, just
Need to regulate and control hydrated reaction of cement process, especially the regulation and control to aquation accelerated period rate of heat release, and then reach diminution
The effect of temperature difference between inside and outside concrete.
Patent CN102674738A discloses a kind of Multifunctional anti-crack additive and preparation method thereof, and its component includes oxidation
Calcium expansive clinker, solubility are 20%-80% commercially available industrial dextrin and flyash, and the anti-crack additive can reduce concrete and put
Hot temperature rise.Because the dextrin in the patent is unmodified dextrin, therefore its regulating effect to the heat of hydration is unsatisfactory.
Patent CN104609768A discloses a kind of hydrated cementitious controlled material, is reacted and made with dextrin by anion-modified dose
.Patent CN104628296A discloses a kind of composite modified heat of hydration controlled material, by starch elder generation and acid catalyst, crosslinking agent
Reaction, product is made with alkenyl succinic acid anhydride reactant again.Above-mentioned patent results show, to water after starch or the modified processing of dextrin
The regulating effect of the mud heat of hydration is greatly improved, but above-mentioned patent is modified preparation process complexity, and the reaction time is longer.
The content of the invention
It is undesirable for the regulating effect of existing hydration heat of cement controlled material, or material preparation process complexity, during reaction
Between it is long the problems such as, the invention discloses a kind of preparation method of simple efficient starch base hydration heat of cement controlled material.
Applicant tests through numerous studies and found, Regulation Mechanism of the starch base hydration heat of cement controlled material to hydrated cementitious
Suction-operated of the hydroxyl to cement granules mainly in starch or dextrin molecule.Using mixed dibasic acid acid anhydride and starch or
Double esterification reaction occurs for the hydroxyl in dextrin molecule, can slow down the rate of dissolution of starch or dextrin under strong alkali environment, and then
Slow down the rate of adsorption of the hydroxyl in cement particle surface, so as to regulate and control the progress of hydration heat reaction.
The invention provides a kind of preparation method of starch base hydration heat of cement controlled material, comprise the steps：
(1) dextrin, starch and mixed dibasic acid acid anhydride are well mixed in high-speed stirring mixer；
(2) by the blend in step (1) through double screw extruder melting extrusion, crush, screening produces product starch base
Hydration heat of cement controlled material；
The mass ratio of dextrin, starch and mixed dibasic acid acid anhydride described in step (1) is 1：(0.1-0.45)：(0.3-1.5)；
Double screw extruder described in step (2) has four sections of heating zones, control first paragraph processing from charging aperture to discharging opening
Temperature is 70-90 DEG C, and second segment processing temperature is 85-120 DEG C, and the 3rd section of processing temperature is 90-130 DEG C, the 4th section of processing temperature
Spend for 100-140 DEG C, screw speed is 80-150r/min, and material residence time in barrel is 8-15min.
Dextrin described in step (1) is commercially available dextrin, and DE values are 4-15, and cold water solubility is 65-100%.
Starch described in step (1) is wheaten starch, cornstarch, waxy corn starch, farina or para arrowroot
One kind in powder.
Mixed dibasic acid acid anhydride described in step (1) is any two in succinic anhydride, glutaric anhydride and phthalic anhydride
Kind.
Product screen size described in step (2) is less than 100 mesh.
Present invention also offers application of the above-mentioned hydration heat of cement controlled material in concrete, its volume is concrete glue
The 0.3-1% of gel material consumption.
It is of the present invention to have the beneficial effect that：
1. the present invention prepares starch base hydration heat of cement controlled material using twin-screw extrusion method, technique is simply efficient, greatly
Width shortens the reaction time, while avoiding the use of solvent in preparation process, reduces harm of the discarded object to environment.
2. the heat release speed of aquation accelerated period and deceleration period can be greatly reduced in heat of hydration controlled material prepared by the inventive method
Rate, and can effectively reduce hydration heat speed peak value more than 80%.Significantly delay aquation induction period different from conventional set retarder, this
The obtained heat of hydration controlled material of invention is not obvious to the retarding action of aquation induction period, therefore to concrete middle and later periods intensity
Substantially do not influence.
Brief description of the drawings
Fig. 1 is influence of the embodiment 3 when volume is 0.3% to hydrated cementitious rate of heat release.
Embodiment
Present disclosure is further described with reference to embodiment, but present disclosure is not limited to reality
Apply the scope of example statement.
Without special instruction in the embodiment of the present invention, the cement used is conch P.O.42.5 cement.Hydrated cementitious is put
The measure of hot speed is carried out using TAM-AIR isothermal calorimeters (TA Instruments), and the water-cement ratio of test cement paste is
0.4, test temperature is 20 DEG C.Compared with being not added with the net slurry of starch base hydration heat of cement controlled material, starch base hydrated cementitious
The performance of hot controlled material is better, then the range of decrease of hydration heat speed peak value is bigger.
In the embodiment of the present invention, test the concrete mix that uses for：Cement 288kg/m3, flyash 72kg/m3, water
195kg/m3, sand 775kg/m3, stone 1165/m3.Sand is the middle sand that modulus of fineness is 2.6, and stone is that particle diameter is 5-20mm
The rubble of continuous grading.
Adiabatic temperature rise of concrete uses Boyuan Science ＆ Technology Development Co. Ltd., Zhoushan City BY-ATC/JR type adiabatic temperature rise instruments,
It is 15 DEG C to test initial temperature.
The setting time of concrete and strength test method are with reference to GB 8076-2008《Concrete admixture》Carry out.
Embodiment 1
By 700gDE values be 4, cold water solubility for 65% commercially available dextrin, 70g wheaten starches, 200g succinic anhydrides and
150g phthalic anhydrides are well mixed in high-speed stirring mixer, add double screw extruder melting extrusion.Twin-screw is squeezed
The processing temperature for going out machine is followed successively by 90 DEG C, 110 DEG C, 120 DEG C, 125 DEG C from charging aperture to discharging opening, and screw speed is 120r/
Min, material residence time in barrel is 10min.Extrudate is crushed, 100 mesh sieves is crossed, produces starch base water of the present invention
Mud heat of hydration controlled material.
Embodiment 2
By 800gDE values be 6, cold water solubility for 72% commercially available dextrin, 160g cornstarch, 180g glutaric anhydrides and
60g succinic anhydrides are well mixed in high-speed stirring mixer, add double screw extruder melting extrusion.Double screw extruder
Processing temperature is followed successively by 70 DEG C, 85 DEG C, 90 DEG C, 100 DEG C from charging aperture to discharging opening, and screw speed is 150r/min, and material exists
The residence time is 8min in barrel.Extrudate is crushed, 100 mesh sieves are crossed, starch base hydration heat of cement of the present invention is produced and adjusts
Control material.
Embodiment 3
It is 9 by 600gDE values, commercially available dextrin, 90g waxy corn starch, 220g succinic anhydrides that cold water solubility is 78%
It is well mixed with 320g phthalic anhydrides in high-speed stirring mixer, adds double screw extruder melting extrusion.Twin-screw
The processing temperature of extruder is followed successively by 90 DEG C, 120 DEG C, 130 DEG C, 140 DEG C from charging aperture to discharging opening, and screw speed is 80r/
Min, material residence time in barrel is 15min.Extrudate is crushed, 100 mesh sieves is crossed, produces starch base water of the present invention
Mud heat of hydration controlled material.
Embodiment 4
It is 12 by 400gDE values, commercially available dextrin, 180g farinas, 300g glutaric anhydrides that cold water solubility is 89%
It is well mixed with 300g succinic anhydrides in high-speed stirring mixer, adds double screw extruder melting extrusion.Twin-screw extrusion
The processing temperature of machine is followed successively by 85 DEG C, 100 DEG C, 110 DEG C, 110 DEG C from charging aperture to discharging opening, and screw speed is 100r/min,
Material residence time in barrel is 12min.Extrudate is crushed, 100 mesh sieves is crossed, produces starch base cement water of the present invention
Change hot controlled material.
Embodiment 5
It is 15 by 500gDE values, commercially available dextrin, 150g tapiocas, 250g glutaric anhydrides that cold water solubility is 100%
It is well mixed with 300g phthalic anhydrides in high-speed stirring mixer, adds double screw extruder melting extrusion.Twin-screw
The processing temperature of extruder is followed successively by 85 DEG C, 120 DEG C, 130 DEG C, 130 DEG C from charging aperture to discharging opening, and screw speed is 80r/
Min, material residence time in barrel is 15min.Extrudate is crushed, 100 mesh sieves is crossed, produces starch base water of the present invention
Mud heat of hydration controlled material.
Benchmark
Without the cement paste or concrete of any additive.
Comparative example 1
Succinic anhydride.
Comparative example 2
Glutaric anhydride.
Comparative example 3
Phthalic anhydride.
Comparative example 4
DE values are 4, and cold water solubility is 65% commercially available dextrin.
Comparative example 5
DE values are 6, and cold water solubility is 72% commercially available dextrin.
Comparative example 6
DE values are 9, and cold water solubility is 78% commercially available dextrin.
Comparative example 7
DE values are 12, and cold water solubility is 89% commercially available dextrin.
Comparative example 8
DE values are 15, and cold water solubility is 100% commercially available dextrin.
Comparative example 9
Wheaten starch.
Comparative example 10
Cornstarch.
Comparative example 11
Waxy corn starch.
Comparative example 12
Farina.
Comparative example 13
Tapioca.
Comparative example 14
It is 9 by 600gDE values, cold water solubility is 78% commercially available dextrin, 90g waxy corn starch and 540g succinic acid
Acid anhydride is well mixed in high-speed stirring mixer, adds double screw extruder melting extrusion.The processing temperature of double screw extruder
90 DEG C, 120 DEG C, 130 DEG C, 140 DEG C are followed successively by from charging aperture to discharging opening, screw speed is 80r/min, and material stops in barrel
It is 15min to stay the time.Extrudate is crushed, 100 mesh sieves is crossed, produces.
Comparative example 15
Embodiment 7 in patent CN104609768A.
1 to 15 couple of hydrated cementitious peak heat release rates of testing example 1 to 5 and comparative example and the influence of concrete performance,
It the results are shown in Table 1.
1 to 15 couple of hydrated cementitious peak heat release rates of the embodiment 1 to 5 of table 1 and comparative example and the influence of concrete performance
As can be seen from Table 1, inhibition of the commercially available dextrin after modified to hydrated cementitious peak heat release rates substantially increases
By force, while the influence to concrete coagulating time and middle and later periods intensity reduces.Before concrete coagulating time is not obviously prolonged
Put, increase volume, inhibition of the starch base hydration heat of cement controlled material to hydration heat speed peak value can be improved.With making
Compared with single dibasic acid anhydride, using starch base hydration heat of cement controlled material made from mixed dibasic acid acid anhydride to hydration heat speed
The inhibition enhancing of rate peak value, highest can effectively reduce hydration heat speed peak value 85.3%, and to the concrete middle and later periods
Intensity does not influence substantially.Twin-screw extrusion method prepares starch base hydration heat of cement controlled material technique simply, greatly shortens
In the reaction time, improve in reaction efficiency, and production process and to be produced without " three wastes ", environmental protection.
Influence of the testing example 3 to Adiabatic temperature rise of concrete, the results are shown in Table 2.
Influence of the embodiment 3 of table 2 to Adiabatic temperature rise of concrete
As can be seen from Table 2, add after embodiment 3, the adiabatic temperature rise climbing speed of concrete substantially slows down, and shows good
Good heat of hydration regulating effect.
Claims (6)
1. a kind of preparation method of starch base hydration heat of cement controlled material, it is characterised in that：Comprise the steps：
（1）Dextrin, starch and mixed dibasic acid acid anhydride are well mixed in high-speed stirring mixer；
（2）By step（1）In blend through double screw extruder melting extrusion, crush, screening produces product starch base cement
Heat of hydration controlled material；
Step（1）Described in dextrin, starch and mixed dibasic acid acid anhydride mass ratio be 1：（0.1-0.45）：（0.3-1.5）；
Step（2）Described in double screw extruder have four sections of heating zones from charging aperture to discharging opening, control first paragraph processing temperature
For 70-90 DEG C, second segment processing temperature is 85-120 DEG C, and the 3rd section of processing temperature is 90-130 DEG C, and the 4th section of processing temperature is
100-140 DEG C, screw speed is 80-150r/min, and material residence time in barrel is 8-15min.
2. preparation method according to claim 1, it is characterised in that step（1）Described in dextrin be commercially available dextrin, DE values
For 4-15, cold water solubility is 65-100%.
3. preparation method according to claim 1, it is characterised in that step（1）Described in starch be wheaten starch, corn
One kind in starch, waxy corn starch, farina or tapioca.
4. preparation method according to claim 1, it is characterised in that step（1）Described in mixed dibasic acid acid anhydride be fourth two
Any two kinds in acid anhydrides, glutaric anhydride and phthalic anhydride.
5. preparation method according to claim 1, it is characterised in that step（2）Described in product screen size be less than 100
Mesh.
6. application of the starch base hydration heat of cement controlled material in concrete described in any one of claim 1 to 5, its feature
It is, the volume of the starch base hydration heat of cement controlled material is the 0.3-1% of concrete gel material consumption.
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| CN107226636B (en) * | 2017-06-06 | 2018-04-06 | 武汉新绿博恩科技有限公司 | A kind of retarder and preparation method thereof |
| CN109776022B (en) * | 2019-03-07 | 2021-06-11 | 东南大学 | Composite controllable hydration cement-based material and application thereof |
| CN112830708B (en) * | 2021-01-19 | 2022-07-19 | 中建商品混凝土有限公司 | Efficient self-compensation hydration heat regulating agent and preparation method and application thereof |
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| CN104609767A (en) * | 2015-02-05 | 2015-05-13 | 江苏苏博特新材料股份有限公司 | Cement hydration rate regulating material as well as preparation method and application of cement hydration rate regulating material |
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