CN108821636A - A kind of preparation method of cement hardener - Google Patents
A kind of preparation method of cement hardener Download PDFInfo
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- CN108821636A CN108821636A CN201810798706.5A CN201810798706A CN108821636A CN 108821636 A CN108821636 A CN 108821636A CN 201810798706 A CN201810798706 A CN 201810798706A CN 108821636 A CN108821636 A CN 108821636A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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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
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present invention relates to a kind of preparation methods of cement hardener, belong to construction material preparation technical field.Beta-cyclodextrin is modified starch by the present invention,Beta-cyclodextrin is polymerized by 7 D- glucopyranoses,Vestibule with similar cone,The present invention is modified stalk using maleic anhydride,Make to introduce double bond and carboxylic acid group on stalk molecule chain,Also mixed with water-absorbing resin,There is carboxyl in these resins,Hydroxyl,Amide groups and sulfonic group etc.,The present invention is mixed using maleic anhydride modified stalk with diatomite,Diatomite has orderly,The big microcellular structure of porosity,The volume of micropore is big simultaneously,A large amount of modified straw particle can be adsorbed in diatomite micropore,With the carboxyl that maleic anhydride is introduced in modified straw particle,Make to avoid that agglomeration occurs between organic molecule,Increase each intermolecular and extraneous contact area,To the more sufficiently efficient moisture absorbed in cement,Reinforce rapid hardening effect,It has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of cement hardener, belong to construction material preparation technical field.
Background technique
Accelerator is to mix the additive that concrete can be made to condense hardening rapidly in concrete.Powdery solid, doping level
Cement consumption 2%~3% in concrete is only accounted for, can but make concrete pre-hardening in 5min, final set in 10min.1h just can produce by force
Degree, 1d intensity improves 2~3 times, but later strength can decline.The rapid hardening early strength function mechanism of accelerator is the gypsum made in cement
Become Na2SO4, deferred action is lost, to promote the rapid aquation of C3A, and its hydrated product crystal is precipitated in the solution, causes
Cement slurry quick solidification.To achieve the purpose that concrete rapid condensation in repairing or roadway.Be in construction of shotcrete method not
The additive that can lack.Their effect is the hydration and hardening for accelerating cement, forms enough intensity in a short period of time, with
Guarantee the requirement of special construction.Accelerator is mainly used for mine working, railway tunnel, diversion culvert, underground engineering.
Accelerator mainly has two class of inorganic salts and organic species.The common accelerator in China is inorganic salts, main type
Number there are I type of Red Star, 7 II, 728 types, 8604 types etc..I type accelerator of Red Star is by aluminum oxide clinker, sodium carbonate, quick lime by quality
1：1：A kind of powder that 0.5 ratio is formulated, moderate dosage are the 2.5%~4.0% of cement quality.7 II type accelerators
It is aluminum oxide clinker and anhydrous gypsum in mass ratio 3：1 cooperation powder forms, and moderate dosage is the 3%~5% of cement quality.
It is seldom applied in construction of shotcrete before the alkaline earth metal carbonate or hydroxide of powdery.They become
This kind of most common accelerator of concrete, only when large dosage incorporation, influence can be just observed.This accelerator and water
The reaction of mud is mainly influenced by chemistry of cement ingredient, fineness and mineral additive and environment temperature.Silicate base sodium metasilicate, silicon
Sour potassium class accelerator is mainly used for wet-mix shotcrete, they are usually all liquid, and volume is very big.Sodium aluminate, aluminic acid
Potassium aluminate class accelerator not only can with dry-mixed but also can be used for wet mixing gunite concrete engineering, common dose is generally 2.5%~
5.5%.Alkali-free liquid accelerator：Alkali-free liquid setting accelerator, its related application report also very rare.This kind of coagulant can solve
The common problem of certainly some alkaline accelerators, such as harm to underground construction environment, the harm of alkali, in use process
The harm of high ph-values and loss etc. to gunite concrete later strength.
Current existing cement hardener rapid hardening is ineffective, slow so as to cause the speed that thes cement solidifies, and keeps later strength poor.
Therefore, inventing a kind of fireballing cement hardener of rapid hardening has positive effect to construction material preparation technical field.
Summary of the invention
The technical problems to be solved by the invention：It is ineffective for current accelerator rapid hardening, so as to cause theing cement solidifies
Slow-footed defect provides a kind of preparation method of cement hardener.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
A kind of preparation method of cement hardener, it is characterised in that specifically preparation step is：
（1）By starch and sodium hydroxide solution in mass ratio 1:4 are stirred, and constant temperature stands 24~26h after mixing, throw after standing
Enter to be centrifuged in centrifuge 4~8 times, be centrifuged 15~20min every time, removes upper layer impurity, be washed with distilled water 3~5 times and be put into
Pretreatment product is dried to obtain in baking oven；
（2）According to parts by weight, 15~18 parts of above-mentioned pretreatment products, 2.5~2.8 parts of beta-cyclodextrins and 24~28 parts of steamings are weighed
Distilled water is put into beaker, and beaker is put into oscillator and is vibrated, is put into freeze drier and crystallizes after oscillation, powder is put into after crystallization
It crushed 150 meshes in broken machine, modified starch be made；
（3）By above-mentioned modified starch and water in mass ratio 1:In 10 investment beakers, it is mixed with blender and mixed emulsion is made,
According to parts by weight, 25~28 parts of mixed emulsions, 2.5~2.8 parts of diatomite, 16~19 parts of acrylic acid and 10~13 parts of hydrogen are weighed
Sodium hydroxide solution puts into three-necked flask and 60~70min is mixed with the revolving speed of 400~450r/min with blender, has stirred
Three-necked flask is put into 2~3h of radiation under ultraviolet light after, modified-reaction liquid is made, it is spare；
（4）By stalk and N, N- DMF solution in mass ratio 1:In 10 investment single-necked flasks, single-necked flask is put into super
It is vibrated in sonication instrument, solidliquid mixture is made, single-necked flask is put into water-bath, it is mixed that solid-liquid is added into single-necked flask
The maleic anhydride solution of amount of substance 15~20% is closed, 4~6h of isothermal reaction is obtained by filtration filter residue, successively uses dehydrated alcohol after reaction
With distillation water washing 3~5 times, it is put into baking oven and dries obtained modified straw；
（5）Above-mentioned modified straw is put into grinder and is ground, after grinding with distilled water in mass ratio 1:10 four mouthfuls of mixing investments
In flask, four-hole boiling flask is placed in isothermal reaction in water-bath, reaction suspension is made and weighs 15~18 according to parts by weight
In part reaction suspension, 1.0~1.5 parts of sodium hydrogensulfites, 12~14 parts of acrylic acid and 8~10 parts of acrylamides investment beakers,
4~5h is stirred with the revolving speed constant temperature of 200~300r/min in the water-bath that temperature is 55~60 DEG C, ethanol washing 5 is used after stirring
It~8 times, with acetone soak and is put into Soxhlet extractor extracting after washing and obtains filter cake, filter cake is put into baking oven and is dried, is made
Obtain reaction product；
（6）By above-mentioned reaction product and spare modified-reaction liquid in mass ratio 1:It, will be in reaction kettle in 3 mixing investment reaction kettles
Temperature, which increases, to be mixed, and is placed in oven and dried after stirring, cement hardener is made in natural cooling.
Step（1）Described in the mass fraction of sodium hydroxide solution be 5~8%, the centrifugal rotational speed of centrifuge is 2800~
3000r/min, the temperature in baking oven are 105~110 DEG C, and drying time is 2~3h.
Step（2）Described in oscillator in temperature be 90~95 DEG C, duration of oscillation be 30~40min, freeze-drying
The temperature of machine is 4~8 DEG C, and crystallization time is 2~3h.
Step（3）Described in blender revolving speed be 400~450r/min, mixing time be 30~40min, hydrogen
The mass fraction of sodium hydroxide solution is 7~10%.
Step（4）Described in N, the mass fraction of N- DMF solution is 15~20%, in supersonic oscillations instrument
Frequency be 30~35kHz, the sonic oscillation time is 80~100min, and the temperature in water-bath is 80~90 DEG C, maleic anhydride
The mass fraction of solution is 10~20%.
Step（5）Described in water-bath bath temperature be 80~85 DEG C, the isothermal reaction time be 30~40min, dry
Temperature in case is 60~65 DEG C.
Step（6）Described in reaction kettle in temperature be increased to 60~70 DEG C, the revolving speed of mixing is 600~700r/
Min, mixing time are 12~13h, and the temperature in baking oven is 120~130 DEG C, and drying time is 5~7h.
The method have the benefit that：
（1）The present invention first pre-processes starch under alkaline condition, and beta-cyclodextrin is added and changes to pretreated starch
Property, then modified starch and acrylic acid and diatomite are mixed to prepare modified-reaction liquid, then by stalk and N, N- dimethylformamide
Mixing adds maleic anhydride and is modified to stalk, and modified stalk and acrylic acid and acrylamide are mixed to prepare instead
Product is answered, finally mixes reaction product with modified-reaction liquid, up to high-efficiency cement accelerator after drying, the present invention pastes β-ring
Essence is modified starch, and beta-cyclodextrin is polymerized by 7 D- glucopyranoses, has the vestibule of similar cone, vestibule
Amylum grain can be coated, forms complexing product with amylum grain, and keeps starch molecule not easy to reunite in crystallization, at scattered shape
Distribution, while being formed by outside conical vestibule with water imbibition, the moisture in cement can be absorbed, to reach rapid hardening effect
Fruit, the present invention are modified stalk using maleic anhydride, make to introduce double bond and carboxylic acid group on stalk molecule chain, also with water suction
Resin mixes, and has carboxyl, hydroxyl, amide groups and sulfonic group etc. in these resins, these groups help to absorb moisture, makes water
Moisture absorption speed in mud increases further to reach rapid hardening effect；
（2）The present invention is mixed using maleic anhydride modified stalk with diatomite, and diatomite has that orderly, porosity is big
Microcellular structure, while the volume of micropore is big, therefore specific surface area is very big, so that adsorption effect is enhanced, in diatomite micropore
A large amount of modified straw particle, the carboxyl for having maleic anhydride introduced in modified straw particle, while diatomite can be adsorbed
Filling has the molecular resin of a large amount of hydrophilic radicals in micropore, makes to avoid that agglomeration occurs between organic molecule, increases each point
Reinforce rapid hardening effect to more sufficiently efficiently absorb the moisture in cement with extraneous contact area between son, have wide
Application prospect.
Specific embodiment
The sodium hydroxide solution in mass ratio 1 for being 5~8% by starch and mass fraction:4 are stirred, and constant temperature is quiet after mixing
24~26h is set, is put into centrifuge after standing, centrifugation 4~8 times under conditions of centrifugal rotational speed is 2800~3000r/min, often
15~20min of secondary centrifugation removes upper layer impurity, is washed with distilled water 3~5 times and is put into the baking oven that temperature is 105~110 DEG C
Dry 2~3h obtains pretreatment product；According to parts by weight, 15~18 parts of above-mentioned pretreatment products, 2.5~2.8 parts of β-are weighed
In cyclodextrin and 24~28 parts of distilled water investment beakers, beaker is put into oscillator, under conditions of temperature is 90~95 DEG C
30~40min is vibrated, is put into freeze drier after oscillation, 2~3h is crystallized under conditions of temperature is 4~8 DEG C, is put after crystallization
Enter and crushed 150 meshes in pulverizer, modified starch is made；By above-mentioned modified starch and water in mass ratio 1:10 investment beakers
In, 30~40min is mixed with the revolving speed of 400~450r/min with blender, mixed emulsion is made, according to parts by weight, claimed
Taking 25~28 parts of mixed emulsions, 2.5~2.8 parts of diatomite, 16~19 parts of acrylic acid and 10~13 parts of mass fractions is 7~10%
Sodium hydroxide solution investment three-necked flask in blender 60~70min is mixed with the revolving speed of 400~450r/min, stir
Three-necked flask is put into 2~3h of radiation under ultraviolet light after the completion of mixing, modified-reaction liquid is made, it is spare；By stalk and mass fraction
For 15~20% N, N- DMF solution in mass ratio 1:In 10 investment single-necked flasks, single-necked flask is put into ultrasonic wave
80~100min is vibrated with the frequency ultrasound of 30~35kHz in shaker, solidliquid mixture is made, single-necked flask is put into temperature
It is 10~20% for the mass fraction of solidliquid mixture quality 15~20% in 80~90 DEG C of water-baths, is added into single-necked flask
Maleic anhydride solution, filter residue is obtained by filtration in 4~6h of isothermal reaction after reaction, successively with dehydrated alcohol and distillation water washing 3~
It 5 times, is put into baking oven and dries obtained modified straw；Above-mentioned modified straw is put into grinder and is ground, after grinding with distilled water
In mass ratio 1:In 10 mixing investment four-hole boiling flasks, four-hole boiling flask is placed in the water-bath that bath temperature is 80~85 DEG C, it is permanent
Reaction suspension is made after 30~40min of temperature reaction and weighs 15~18 parts of reactions suspensions, 1.0~1.5 according to parts by weight
In part sodium hydrogensulfite, 12~14 parts of acrylic acid and 8~10 parts of acrylamides investment beakers, the water-bath for being 55~60 DEG C in temperature
In 4~5h stirred with the revolving speed constant temperature of 200~300r/min, used ethanol washing 5~8 times after stirring, acetone soak used after washing
And be put into extracting in Soxhlet extractor and obtain filter cake, filter cake is put into the baking oven that temperature is 60~65 DEG C and is dried, reaction is made
Product；By above-mentioned reaction product and spare modified-reaction liquid in mass ratio 1:In 3 mixing investment reaction kettles, by reaction kettle medium temperature
Degree is increased to 60~70 DEG C, and 12~13h is mixed with the revolving speed of 600~700r/min, is put into baking oven after stirring, with
Cement hardener is made in the dry 5~7h of 120~130 DEG C of temperature, natural cooling.
The sodium hydroxide solution in mass ratio 1 for being 5% by starch and mass fraction:4 are stirred, and constant temperature is stood after mixing
For 24 hours, it is put into centrifuge after standing, is centrifuged 4 times under conditions of centrifugal rotational speed is 2800r/min, is centrifuged 15min every time, goes
Except upper layer impurity, it is washed with distilled water 3 times and is put into dry 2h in the baking oven that temperature is 105 DEG C and obtain pretreatment product；By weight
Number meter is measured, weighs in 15 parts of above-mentioned pretreatment products, 2.5 parts of beta-cyclodextrins and 24 parts of distilled water investment beakers, beaker is put
Enter in oscillator, 30min is vibrated under the conditions of at a temperature of 90 °C, is put into freeze drier after oscillation, is 4 DEG C in temperature
Under the conditions of crystallize 2h, be put into after crystallization in pulverizer and crushed 150 meshes, be made modified starch；By above-mentioned modified starch and water
In mass ratio 1:In 10 investment beakers, 30min is mixed with the revolving speed of 400r/min with blender, mixed emulsion is made, by weight
Number meter is measured, the sodium hydroxide that 25 parts of mixed emulsions, 2.5 parts of diatomite, 16 parts of acrylic acid and 10 parts of mass fractions are 7% is weighed
Solution puts into three-necked flask and 60min is mixed with the revolving speed of 400r/min with blender, by three-necked flask after the completion of stirring
It is put under ultraviolet light and radiates 2h, modified-reaction liquid is made, it is spare；The N for being 15% by stalk and mass fraction, N- dimethylformamide
Solution in mass ratio 1:In 10 investment single-necked flasks, single-necked flask is put into the frequency ultrasound in supersonic oscillations instrument with 30kHz
80min is vibrated, solidliquid mixture is made, single-necked flask is put into the water-bath that temperature is 80 DEG C, is added into single-necked flask
Filter residue is obtained by filtration after reaction in the maleic anhydride solution that the mass fraction of solidliquid mixture quality 15% is 10%, isothermal reaction 4h,
Successively with dehydrated alcohol and distillation water washing 3 times, it is put into baking oven and dries obtained modified straw；Above-mentioned modified straw is put into and is ground
Ground in grinding machine, after grinding with distilled water in mass ratio 1:In 10 mixing investment four-hole boiling flasks, four-hole boiling flask is placed in water-bath temperature
Is reaction suspension is made in degree in 80 DEG C of water-bath, after isothermal reaction 30min, according to parts by weight, it is outstanding to weigh 15 parts of reactions
In turbid, 1.0 parts of sodium hydrogensulfites, 12 parts of acrylic acid and 8 parts of acrylamides investment beakers, in the water-bath that temperature is 55 DEG C with
The revolving speed constant temperature of 200r/min stirs 4h, uses ethanol washing 5 times after stirring, with acetone soak and is put into Soxhlet extractor after washing
Middle extracting obtains filter cake, and filter cake is put into the baking oven that temperature is 60 DEG C and is dried, and reaction product is made；By above-mentioned reaction product with
Spare modified-reaction liquid in mass ratio 1:In 3 mixing investment reaction kettles, temperature in reaction kettle is increased to 60 DEG C, and with
12h is mixed in the revolving speed of 600r/min, is put into baking oven after stirring, and with the dry 5h of 120 DEG C of temperature, water is made in natural cooling
Mud accelerator.
The sodium hydroxide solution in mass ratio 1 for being 7% by starch and mass fraction:4 are stirred, and constant temperature is stood after mixing
25h is put into centrifuge after standing, is centrifuged 6 times under conditions of centrifugal rotational speed is 2900r/min, is centrifuged 17min every time, goes
Except upper layer impurity, it is washed with distilled water 4 times and is put into dry 2.5h in the baking oven that temperature is 107 DEG C and obtain pretreatment product；It presses
Parts by weight meter weighs in 17 parts of above-mentioned pretreatment products, 2.7 parts of beta-cyclodextrins and 26 parts of distilled water investment beakers, by beaker
It is put into oscillator, vibrates 35min under conditions of temperature is 92 DEG C, be put into freeze drier after oscillation, be 6 DEG C in temperature
Under conditions of crystallize 2.5h, be put into after crystallization in pulverizer and crushed 150 meshes, be made modified starch；By above-mentioned modified starch
With water in mass ratio 1:In 10 investment beakers, 35min is mixed with the revolving speed of 420r/min with blender, mixed emulsion is made,
According to parts by weight, the hydrogen-oxygen that 27 parts of mixed emulsions, 2.7 parts of diatomite, 18 parts of acrylic acid and 12 parts of mass fractions are 8% is weighed
Change in sodium solution investment three-necked flask and 65min is mixed with the revolving speed of 420r/min with blender, by three mouthfuls after the completion of stirring
Flask is put under ultraviolet light and radiates 2.5h, and modified-reaction liquid is made, spare；The N for being 18% by stalk and mass fraction, N- diformazan
Base amide solution in mass ratio 1:In 10 investment single-necked flasks, single-necked flask is put into the frequency in supersonic oscillations instrument with 32kHz
Solidliquid mixture is made in rate sonic oscillation 90min, single-necked flask is put into the water-bath that temperature is 85 DEG C, to single-necked flask
The maleic anhydride solution that the middle mass fraction that solidliquid mixture quality 17% is added is 15%, isothermal reaction 5h are filtered after reaction
To filter residue, successively with dehydrated alcohol and distillation water washing 4 times, it is put into baking oven and dries obtained modified straw；By above-mentioned modified straw
Stalk is put into grinder and grinds, after grinding with distilled water in mass ratio 1:In 10 mixing investment four-hole boiling flasks, four-hole boiling flask is set
Reaction suspension is made in the water-bath that bath temperature is 82 DEG C, after isothermal reaction 35min and weighs 17 according to parts by weight
It is 57 DEG C in temperature in part reaction suspension, 1.2 parts of sodium hydrogensulfites, 13 parts of acrylic acid and 9 parts of acrylamides investment beakers
4.5h is stirred with the revolving speed constant temperature of 250r/min in water-bath, is used ethanol washing 7 times after stirring, with acetone soak and is put into after washing
Extracting obtains filter cake in Soxhlet extractor, and filter cake is put into the baking oven that temperature is 62 DEG C and is dried, and reaction product is made；It will be above-mentioned
Reaction product and spare modified-reaction liquid in mass ratio 1:In 3 mixing investment reaction kettles, temperature in reaction kettle is increased to 65
DEG C, and 12.5h is mixed with the revolving speed of 650r/min, and it is put into baking oven after stirring, it is natural with the dry 6h of 125 DEG C of temperature
Cooling obtained cement hardener.
By the sodium hydroxide solution in mass ratio 1 of starch and mass fraction 8%:4 are stirred, and constant temperature is stood after mixing
26h is put into centrifuge after standing, is centrifuged 8 times under conditions of centrifugal rotational speed is 3000r/min, is centrifuged 20min every time, goes
Except upper layer impurity, it is washed with distilled water 5 times and is put into dry 3h in the baking oven that temperature is 110 DEG C and obtain pretreatment product；By weight
Number meter is measured, weighs in 18 parts of above-mentioned pretreatment products, 2.8 parts of beta-cyclodextrins and 28 parts of distilled water investment beakers, beaker is put
Enter in oscillator, vibrate 40min under conditions of temperature is 95 DEG C, be put into freeze drier after oscillation, is 8 DEG C in temperature
Under the conditions of crystallize 3h, be put into after crystallization in pulverizer and crushed 150 meshes, be made modified starch；By above-mentioned modified starch and water
In mass ratio 1:In 10 investment beakers, 40min is mixed with the revolving speed of 450r/min with blender, mixed emulsion is made, by weight
Number meter is measured, the sodium hydroxide that 28 parts of mixed emulsions, 2.8 parts of diatomite, 19 parts of acrylic acid and 13 parts of mass fractions are 10% is weighed
Solution puts into three-necked flask and 70min is mixed with the revolving speed of 450r/min with blender, by three-necked flask after the completion of stirring
It is put under ultraviolet light and radiates 3h, modified-reaction liquid is made, it is spare；The N for being 20% by stalk and mass fraction, N- dimethylformamide
Solution in mass ratio 1:In 10 investment single-necked flasks, single-necked flask is put into the frequency ultrasound in supersonic oscillations instrument with 35kHz
100min is vibrated, solidliquid mixture is made, single-necked flask is put into water-bath at a temperature of 90 °C, is added into single-necked flask
Filter residue is obtained by filtration after reaction in the maleic anhydride solution that the mass fraction of solidliquid mixture quality 20% is 20%, isothermal reaction 6h,
Successively with dehydrated alcohol and distillation water washing 5 times, it is put into baking oven and dries obtained modified straw；Above-mentioned modified straw is put into and is ground
Ground in grinding machine, after grinding with distilled water in mass ratio 1:In 10 mixing investment four-hole boiling flasks, four-hole boiling flask is placed in water-bath temperature
Is reaction suspension is made in degree in 85 DEG C of water-bath, after isothermal reaction 40min, according to parts by weight, it is outstanding to weigh 18 parts of reactions
In turbid, 1.5 parts of sodium hydrogensulfites, 14 parts of acrylic acid and 10 parts of acrylamide investment beakers, in the water-bath that temperature is 60 DEG C
5h is stirred with the revolving speed constant temperature of 300r/min, is used ethanol washing 8 times after stirring, with acetone soak and is put into soxhlet type after washing
Extracting obtains filter cake in device, and filter cake is put into the baking oven that temperature is 65 DEG C and is dried, and reaction product is made；By above-mentioned reaction product
With spare modified-reaction liquid in mass ratio 1:In 3 mixing investment reaction kettles, temperature in reaction kettle is increased to 70 DEG C, and with
13h is mixed in the revolving speed of 700r/min, is put into baking oven after stirring, and with the dry 7h of 130 DEG C of temperature, water is made in natural cooling
Mud accelerator.
The cement hardener that comparative example is produced with Yancheng company is as a comparison case to cement hardener produced by the present invention
Performance detection is carried out with the cement hardener in comparative example, testing result is as shown in table 1：
Test method：
Presetting period and final setting time are tested：According to JC477-2005《Gunite concrete accelerator》Standard, test water mud
(GB8076-2008), accelerator volume is the 6% of cement quality.
Strength test：According to JC477-2005《Gunite concrete accelerator》Standard, test water mud (GB8076-
2008), accelerator volume is the 6% of cement quality.
1 accelerator performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example |
| Presetting period（min） | 2.8 | 2.6 | 2.3 | 10.5 |
| Final setting time（min） | 6.6 | 6.4 | 6.2 | 30.8 |
| 1d compression strength（MPa） | 12.2 | 12.4 | 12.5 | 5.2 |
| 28d compressive strength rate（%） | 103.9 | 104.2 | 104.5 | 85 |
According to the cement hardener rapid hardening effect produced by the present invention of data among the above, the presetting period is short, and final setting time is short, by force
Degree is high, has broad application prospects.
Claims (7)
1. a kind of preparation method of cement hardener, it is characterised in that specifically preparation step is：
（1）By starch and sodium hydroxide solution in mass ratio 1:4 are stirred, and constant temperature stands 24~26h after mixing, throw after standing
Enter to be centrifuged in centrifuge 4~8 times, be centrifuged 15~20min every time, removes upper layer impurity, be washed with distilled water 3~5 times and be put into
Pretreatment product is dried to obtain in baking oven；
（2）According to parts by weight, 15~18 parts of above-mentioned pretreatment products, 2.5~2.8 parts of beta-cyclodextrins and 24~28 parts of steamings are weighed
Distilled water is put into beaker, and beaker is put into oscillator and is vibrated, is put into freeze drier and crystallizes after oscillation, powder is put into after crystallization
It crushed 150 meshes in broken machine, modified starch be made；
（3）By above-mentioned modified starch and water in mass ratio 1:In 10 investment beakers, it is mixed with blender and mixed emulsion is made,
According to parts by weight, 25~28 parts of mixed emulsions, 2.5~2.8 parts of diatomite, 16~19 parts of acrylic acid and 10~13 parts of hydrogen are weighed
Sodium hydroxide solution puts into three-necked flask and 60~70min is mixed with the revolving speed of 400~450r/min with blender, has stirred
Three-necked flask is put into 2~3h of radiation under ultraviolet light after, modified-reaction liquid is made, it is spare；
（4）By stalk and N, N- DMF solution in mass ratio 1:In 10 investment single-necked flasks, single-necked flask is put into super
It is vibrated in sonication instrument, solidliquid mixture is made, single-necked flask is put into water-bath, it is mixed that solid-liquid is added into single-necked flask
The maleic anhydride solution of amount of substance 15~20% is closed, 4~6h of isothermal reaction is obtained by filtration filter residue, successively uses dehydrated alcohol after reaction
With distillation water washing 3~5 times, it is put into baking oven and dries obtained modified straw；
（5）Above-mentioned modified straw is put into grinder and is ground, after grinding with distilled water in mass ratio 1:10 four mouthfuls of mixing investments
In flask, four-hole boiling flask is placed in isothermal reaction in water-bath, reaction suspension is made and weighs 15~18 according to parts by weight
In part reaction suspension, 1.0~1.5 parts of sodium hydrogensulfites, 12~14 parts of acrylic acid and 8~10 parts of acrylamides investment beakers,
4~5h is stirred with the revolving speed constant temperature of 200~300r/min in the water-bath that temperature is 55~60 DEG C, ethanol washing 5 is used after stirring
It~8 times, with acetone soak and is put into Soxhlet extractor extracting after washing and obtains filter cake, filter cake is put into baking oven and is dried, is made
Obtain reaction product；
（6）By above-mentioned reaction product and spare modified-reaction liquid in mass ratio 1:It, will be in reaction kettle in 3 mixing investment reaction kettles
Temperature, which increases, to be mixed, and is placed in oven and dried after stirring, cement hardener is made in natural cooling.
2. a kind of preparation method of cement hardener according to claim 1, it is characterised in that：Step（1）Described in
The mass fraction of sodium hydroxide solution is 5~8%, and the centrifugal rotational speed of centrifuge is 2800~3000r/min, the temperature in baking oven
It is 105~110 DEG C, drying time is 2~3h.
3. a kind of preparation method of cement hardener according to claim 1, it is characterised in that：Step（2）Described in
Temperature in oscillator is 90~95 DEG C, and duration of oscillation is 30~40min, and the temperature of freeze drier is 4~8 DEG C, when crystallization
Between be 2~3h.
4. a kind of preparation method of cement hardener according to claim 1, it is characterised in that：Step（3）Described in
The revolving speed of blender is 400~450r/min, and mixing time is 30~40min, and the mass fraction of sodium hydroxide solution is 7
~10%.
5. a kind of preparation method of cement hardener according to claim 1, it is characterised in that：Step（4）Described in
N, the mass fraction of N- DMF solution is 15~20%, and the frequency in supersonic oscillations instrument is 30~35kHz, ultrasound
Duration of oscillation is 80~100min, and the temperature in water-bath is 80~90 DEG C, the mass fraction of maleic anhydride solution is 10~
20%。
6. a kind of preparation method of cement hardener according to claim 1, it is characterised in that：Step（5）Described in
The bath temperature of water-bath is 80~85 DEG C, and the isothermal reaction time is 30~40min, and the temperature in baking oven is 60~65 DEG C.
7. a kind of preparation method of cement hardener according to claim 1, it is characterised in that：Step（6）Described in
Temperature is increased to 60~70 DEG C in reaction kettle, and the revolving speed of mixing is 600~700r/min, and mixing time is 12~
13h, the temperature in baking oven are 120~130 DEG C, and drying time is 5~7h.
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Cited By (1)
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| CN116375399A (en) * | 2023-03-22 | 2023-07-04 | 河源市源隆新型环保建材有限公司 | Dry-mixed thin-layer anti-cracking plastering mortar and preparation method thereof |
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