CN109535347A - A kind of preparation method of block water-retaining type concrete admixture - Google Patents
A kind of preparation method of block water-retaining type concrete admixture Download PDFInfo
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- CN109535347A CN109535347A CN201811580927.1A CN201811580927A CN109535347A CN 109535347 A CN109535347 A CN 109535347A CN 201811580927 A CN201811580927 A CN 201811580927A CN 109535347 A CN109535347 A CN 109535347A
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/243—Phosphorus-containing polymers
- C04B24/246—Phosphorus-containing polymers containing polyether side chains
Abstract
The invention belongs to build additive technical field, more particularly to a kind of preparation method of block water-retaining type concrete admixture, include the following steps: that unsaturated polyether monomer A is added in a kettle, unsaturated cross-linking monomer, acrylic acid, L-AA, chain-transferring agent, green vitriol and deionized water, and it is stirred, after material is completely dissolved, hydrogen peroxide is added, continue to stir, after equal 1-3h, it is again stirring for, and unsaturated polyether monomer B is added, unsaturated polyether monomer C, acrylic acid, oxidant and deionized water, heat temperature raising, start that mixed solution I is added dropwise, after 10min, mixed solution II is added dropwise again, hydrogen peroxide and sodium phosphate are added into reaction kettle after being added dropwise for mixed solution I and mixed solution II, and it cools after keeping the temperature 1h, obtain block water-retaining type coagulation Native additive.The present invention can improve the cohesiveness of concrete mix, reduce concrete disintegration, bleeding, Reasonable Regulation And Control concrete work state.
Description
Technical field
The invention belongs to build additive technical field, and in particular to a kind of system of block water-retaining type concrete admixture
Preparation Method.
Background technique
Concrete admixture is widely used in deionized water cement-based material, such as deionized water cement paste, mortar and coagulation
Soil, it is very necessary in engineering construction field and building structure.These concrete admixtures can increase deionization cement matrix
The mobility of material effectively improves the performance of the maturings such as intensity, durability.As concrete is to high performance and more
The direction of functionalization is developed, it is desirable that concrete has high workability, high intensity, high-durability, and is able to satisfy in many special feelings
Application under condition, oneself becomes indispensable component in high performance concrete.
Concrete admixture has excellent dispersion performance, concrete can be made at low dosage to reach preferable stream
Dynamic property can pass free radical copolymerization in principle according to MOLECULE DESIGN and close polymerizable structural unit during the preparation process
At the concrete admixture of predetermined structure and performance, usually by containing carboxylic acid group, sulfonic group, ester group and polyethylene oxide base etc. one
A little monomers with unsaturated group are synthesized by free radicals copolymerization reaction.In the polymerization preparation process of concrete admixture,
Different monomers make molecule with certain Molecular Geometries, special knot to condense together at random or regularly
Structure determines its superior function.Currently, the molecular structure of most concrete admixtures is linear comb structure, generally exist
Steric hindrance effect is weaker in the heterogeneous system of concrete, therefore the dispersibility in deionized water slurry body, slump retaining, guarantor
Deionized water effect and its universality are to be improved.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of system of block water-retaining type concrete admixture is provided
Preparation Method.
Technical scheme is as follows:
By weight:
150-180 parts of unsaturations are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
A, 5-10 parts of polyether monomer unsaturated cross-linking monomers, 10-30 parts of acrylic acid, 0.2-2 parts of L- ascorbic acid, 0.4-0.8 parts of chains turn
Move agent, 0.01-0.05 parts of green vitriols and 100-150 parts of deionized waters；
Start agitating device stirring, temperature controller is controlled at 15-35 DEG C, after material is completely dissolved, is added 1-5 parts
Hydrogen peroxide continues to stir 5min, stops stirring；
It is again started up agitating device after 1-3h, and 20-30 parts of unsaturated polyether monomers B, 5-10 are added into reaction kettle
Part unsaturated polyether monomer C, 3-6 part acrylic acid, 2-5 parts of oxidants and 30-50 parts of deionized waters；
When being heated to 50-65 DEG C, it is added dropwise with Dropping feeder and is gone by 2-5 parts of unsaturated amino compounds and 30-40 parts
The mixed solution I that ionized water is configured to after 10min, then is added dropwise by 0.2-0.5 parts of complex reducing agents, 0.1-0.3 parts of chain tra nsfers
The mixed solution II that agent and 30-40 parts of deionized waters are configured to, mixed solution I should be added dropwise in 0.5-1h, mixed solution
II should be added dropwise in 1-1.5h, and 1-2 is added after being added dropwise in solution I and mixed solution II to be mixed into reaction kettle again
Part hydrogen peroxide and 0.2-0.5 parts of sodium phosphates cool after keeping the temperature 1h to get block water-retaining type concrete admixture is arrived.
Further, unsaturated polyether monomer A includes such as flowering structure (a):
H(OCH2CH2)p(OCH2CH2CH2)qOCH2CH2CR1=CH2 (a)
Wherein, p is integer, and 5≤p≤10；Q is integer, and 1≤q≤2；R1For H or CH3。
Further, unsaturated cross-linking monomer is three acrylic ester of phosphorous acid, allyl phosphonic acid diallyl, triallyl
One of phosphate.
Further, chain-transferring agent is one of thioacetic acid, mercaptopropionic acid, mercaptoethanol.
Further, unsaturated polyether monomer B includes such as flowering structure (b):
CH3CH2O(CH2CH2O)m(CH2CH2CH2O)nCH2CH2OOCH2CR2=CH2 (b)
Wherein, m is integer, and 20≤m≤25；N is integer, and 1≤n≤3；R2For H or CH3。
Further, unsaturated polyether monomer C includes such as flowering structure (c):
CH2=CR3CH2OO(CH2CH2CH2O)x(CH2CH2O)yOCH2CR4=CH2 (c)
Wherein, x is integer, and 1≤x≤2；Y is integer, and 5≤y≤10；R3, R4For H or CH3。
Further, oxidant is one of hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
Further, unsaturated amino compounds areD- allylglycine、2- amino -4- methyl -4- penetenoic acid、2- ammonia Base -3-butenoic acid, one of 2- amino -5- hexenoic acid.
Further, complex reducing agent by weight, has following composition:
2- hydroxyl -2- sulfinatoacetic acid zinc: 40-60%；
2- hydroxyl -2- sulfonatoacetic acid zinc: 1-4%；
L-AA: 1-5%；
It is a kind of in sodium dithionite, potassium hyposulfite or zinc dithionite: 15-35%；
It is a kind of in sodium carbonate, sodium bicarbonate, potassium carbonate or saleratus: 10-20%.
The beneficial effects of the present invention are: using aqueous free radical copolymerization, using unsaturated monomer, initiator,
Chain-transferring agent etc., which is synthesized by two-step process, prepares block polymer, has strong operability, reaction process is easy to control, to anti-
Answer condition responsive low, it is easy to industrialized production the features such as.By the polyethers for introducing different type and length in molecular side chain
Side chain can regulate and control concrete admixture and steric configuration and unfold degree in concrete heterogeneous system；By in molecular backbone
Introducing crosslinked monomer, unsaturated amino compounds etc. can improve the lubricant effect and hydrophilic shape of particle in the multinomial system of concrete
State improves the cohesiveness of concrete mix, reduces concrete disintegration, bleeding, Reasonable Regulation And Control concrete work state.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to solve
The present invention is released, is not intended to limit the present invention.
Wherein, in embodiment 1-4, the ingredient and ratio of used complex reducing agent are as listed in table 1.
1 complex reducing agent ingredient of table and ratio
Embodiment 1
By weight, 150 parts are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
H(OCH2CH2)5OCH2CH2CH2OCH2CH2CH=CH2, 5 parts of three acrylic esters of phosphorous acid, 10 parts of acrylic acid, 0.2 part of L- Vitamin C
Acid, 0.8 part of thioacetic acid, 0.05 part of green vitriol and 100 parts of deionized waters, starting agitating device stirring, thermostat
Controlled at 35 DEG C, after material is completely dissolved, 3 parts of hydrogen peroxide are added, continues to stir 5min, then stops stirring, to
After 1h, it is again started up agitating device, and 25 parts of CH are added into reaction kettle3CH2O(CH2CH2O)20CH2CH2CH2OCH2CH2OOCH2CH=CH2, 5 parts of CH2=CHCH2OO(CH2CH2CH2O)2(CH2CH2O)5OCH2CCH3=CH2,
3 parts of acrylic acid, 5 parts of hydrogen peroxide and 35 parts of deionized waters when being heated to 65 DEG C, start to be added dropwise with Dropping feeder by 2-
5 partsD- allylglycineThe mixed solution I being configured to 35 parts of deionized waters after 10min, then is added dropwise compound by 0.2 part
The mixed solution II that reducing agent, 0.2 part of thioacetic acid and 35 parts of deionized waters are configured to, mixed solution I should be added dropwise in 0.5h
Finish, mixed solution II should be added dropwise in 1h, solution I and mixed solution II to be mixed be added dropwise to complete after again toward reaction kettle
1 part of hydrogen peroxide of middle addition and 0.5 part of sodium phosphate cool after keeping the temperature 1h to get additional to block water-retaining type concrete
Agent.
Embodiment 2
By weight, 160 parts are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
H(OCH2CH2)6(OCH2CH2CH2)2OCH2CH2CCH3=CH2, 6 parts of allyl phosphonic acid diallyls, 30 parts of acrylic acid, 0.5 part
L-AA, 0.8 part of thioacetic acid, 0.03 part of green vitriol and 120 parts of deionized waters, starting agitating device into
Row stirring, thermostat is controlled at 30 DEG C, and after material is completely dissolved, 2 parts of hydrogen peroxide are added, and continues to stir 5min, so
Stop stirring afterwards, after 2h, be again started up agitating device and be stirred, and 26 parts of CH are added into reaction kettle3CH2O
(CH2CH2O)22(CH2CH2CH2O)2CH2CH2OOCH2CH=CH2, 10 parts of CH2=CCH3CH2OOCH2CH2CH2O(CH2CH2O)7OCH2CH=CH2, 4 parts of acrylic acid, 2 parts of ammonium persulfates and 40 parts of deionized waters when being heated to 50 DEG C, start with being added dropwise
Device is added dropwise by 2-5 parts2- amino -4- methyl -4- penetenoic acidThe mixed solution I being configured to 40 parts of deionized waters, to 10min
Afterwards, then the mixed solution II being configured to by 0.5 part of complex reducing agent, 0.1 part of mercaptopropionic acid and 40 parts of deionized waters is added dropwise, mixes
Closing solution I should be added dropwise in 1h, and mixed solution II should be added dropwise in 1.5h, solution I and mixed solution II to be mixed
1.5 parts of hydrogen peroxide and 0.2 part of sodium phosphate is added after being added dropwise to complete into reaction kettle again, cools after keeping the temperature 1h to get arriving
Block water-retaining type concrete admixture.
Embodiment 3
By weight, 170 parts are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
H(OCH2CH2)8(OCH2CH2CH2)3OCH2CH2CCH3=CH2, 10 parts of triallyl phosphates, 20 parts of acrylic acid, 1 part of L- is anti-bad
Hematic acid, 0.4 part of mercaptopropionic acid, 0.01 part of green vitriol and 150 parts of deionized waters, starting agitating device are stirred,
Thermostat is controlled at 15 DEG C, and after material is completely dissolved, 1 part of hydrogen peroxide is added, and continues to stir 5min, then stop
Stirring, after 3h, is again started up agitating device and is stirred, and 20 parts of CH are added into reaction kettle3CH2O(CH2CH2O)23
(CH2CH2CH2O)2CH2CH2OOCH2CH=CH2, 8 parts of CH2=CCH3CH2OO(CH2CH2CH2O)2(CH2CH2O)10OCH2CCH3=
CH2, 5 parts of acrylic acid, 3 parts of sodium peroxydisulfates and 30 parts of deionized waters when being heated to 55 DEG C, start to be added dropwise with Dropping feeder
By 2-5 parts2- amino -3-butenoic acidThe mixed solution I being configured to 30 parts of deionized waters, after 10min, then is added dropwise by 0.4
The mixed solution II that part complex reducing agent, 0.1 part of mercaptoethanol and 30 parts of deionized waters are configured to, mixed solution I should be in 0.8h
It is inside added dropwise, mixed solution II should be added dropwise in 1h, and solution I and mixed solution II to be mixed are past again after being added dropwise to complete
1.8 parts of hydrogen peroxide and 0.4 part of sodium phosphate are added in reaction kettle, cools after keeping the temperature 1h to get block water-retaining type coagulation is arrived
Native additive.
Embodiment 4
By weight, 180 parts are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
H(OCH2CH2)10(OCH2CH2CH2)2OCH2CH2CH=CH2, 8 parts of triallyl phosphates, 15 parts of acrylic acid, 2 parts of L- Vitamin Cs
Acid, 0.5 part of mercaptoethanol, 0.04 part of green vitriol and 135 parts of deionized waters, starting agitating device are stirred, control
Warm device is controlled at 25 DEG C, and after material is completely dissolved, 5 parts of hydrogen peroxide are added, and continues to stir 5min, then stops stirring
It mixes, after 1h, is again started up agitating device and is stirred, and 30 parts of CH are added into reaction kettle3CH2O(CH2CH2O)25
(CH2CH2CH2O)3CH2CH2OOCH2CCH3=CH2, 10 parts of CH2=CHCH2OOCH2CH2CH2O(CH2CH2O)9OCH2CH=CH2,
6 parts of acrylic acid, 4 parts of potassium peroxydisulfates and 50 parts of deionized waters when being heated to 60 DEG C, start to be added dropwise with Dropping feeder by 2-5
The mixed solution I that part 2- amino -5- hexenoic acid and 30 parts of deionized waters are configured to after 10min, then is added dropwise multiple by 0.3 part
The mixed solution II that reducing agent, 0.3 part of mercaptoethanol and 40 parts of deionized waters are configured to is closed, mixed solution I should be added dropwise in 1h
It finishes, mixed solution II should be added dropwise in 1.5h, past reaction again after solution I and mixed solution II to be mixed are added dropwise to complete
2 parts of hydrogen peroxide and 0.3 part of sodium phosphate are added in kettle, cools after keeping the temperature 1h to get additional to block water-retaining type concrete
Agent.
By the embodiment 1-4 sample synthesized and comparative sample (commercial standard type high-performance water reducing agent, HPWR-S),
It is " common according to GB/T 50080-2016 " Standard for test methods of properties of ordinary concrete mixture standard " and GB/T 50081-2016
Mechanical performance of concrete test method standard " carry out concrete mixture characteristic test method and properties of hardened concrete test.
The main raw material(s) that performance test uses:
Cement (C): 42.5 ordinary portland cement of P.O, crop field Hong Shi Cement Co., Ltd；
Flyash (FA): II grade of flyash, Xiamen Sha Ye trade Co., Ltd；
Miberal powder (SL): S95 grades, Fujian Triratna Iron And Steel Co., Ltd；
Sand (S): fineness modulus 2.8, clay content is less than 1%, Xiamen Wan Xiangtong Industrial Co., Ltd.；
Stone (G): 5-25mm graded broken stone, Xiamen is along building materials Co., Ltd of heap of stone；
Test water (W): tap water meets the regulation of JGJ 63-2006 " concrete water standard ".
The concrete mix that performance test uses is shown in Table 2, and performance test data is shown in Table 3.
2 concrete mix of table
| Raw material | C | FA | SL | S | G | W |
| Dosage/(kg/m3) | 280 | 70 | 70 | 740 | 1020 | 162 |
3 concrete test performance of table
From the performance test data of table 3, it can be seen that technical solution of the present invention has the effect of obvious water conservation, anti-isolation
Fruit.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, therefore, as long as with
Any modifications, equivalent replacements, and improvements made by present specification etc., should be included in protection scope of the present invention it
It is interior.
Claims (9)
1. a kind of preparation method of block water-retaining type concrete admixture, characterized by the following steps:
By weight:
150-180 parts of unsaturated polyether lists are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
A, 5-10 parts of body unsaturated cross-linking monomers, 10-30 parts of acrylic acid, 0.2-2 parts of L-AAs, 0.4-0.8 parts of chain-transferring agents,
0.01-0.05 parts of green vitriols and 100-150 parts of deionized waters；
Start the agitating device stirring, and the thermostat after material is completely dissolved, adds controlled at 15-35 DEG C
Enter 1-5 parts of hydrogen peroxide, continues to stir 5min, then stop stirring；
After equal 1-3h, it is again started up the agitating device stirring, and 20-30 parts of unsaturated polyether lists are added into the reaction kettle
B, 5-10 parts of unsaturated polyether monomer C, 3-6 part acrylic acid of body, 2-5 parts of oxidants and 30-50 parts of deionized waters；
When being heated to 50-65 DEG C, start to be added dropwise with the Dropping feeder by 2-5 parts of unsaturated amino compounds and 30-40
The mixed solution I that part deionized water is configured to, after 10min, then is added dropwise by 0.2-0.5 parts of complex reducing agents, 0.1-0.3 parts of chains
The mixed solution II that transfer agent and 30-40 parts of deionized waters are configured to, the mixed solution I are added dropwise in 0.5-1h, institute
It states mixed solution II to be added dropwise in 1-1.5h, the mixed solution I and the mixed solution II are added dropwise afterwards toward described
1-2 parts of hydrogen peroxide and 0.2-0.5 parts of sodium phosphates are added in reaction kettle, and cool after keeping the temperature 1h to get block water conservation is arrived
Type concrete admixture.
2. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated polyether monomer A includes such as flowering structure (a):
H(OCH2CH2)p(OCH2CH2CH2)qOCH2CH2CR1=CH2 (a)
Wherein, p is integer, and 5≤p≤10；Q is integer, and 1≤q≤2；R1For H or CH3。
3. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated cross-linking monomer is one of three acrylic ester of phosphorous acid, allyl phosphonic acid diallyl, triallyl phosphate.
4. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Chain-transferring agent is one of thioacetic acid, mercaptopropionic acid, mercaptoethanol.
5. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated polyether monomer B includes such as flowering structure (b):
CH3CH2O(CH2CH2O)m(CH2CH2CH2O)nCH2CH2OOCH2CR2=CH2 (b)
Wherein, m is integer, and 20≤m≤25；N is integer, and 1≤n≤3；R2For H or CH3。
6. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated polyether monomer C includes such as flowering structure (c):
CH2=CR3CH2OO(CH2CH2CH2O)x(CH2CH2O)yOCH2CR4=CH2 (c)
Wherein, x is integer, and 1≤x≤2；Y is integer, and 5≤y≤10；R3, R4For H or CH3。
7. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Oxidant is one of hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
8. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated amino compounds areD- allylglycine、2- amino -4- methyl -4- penetenoic acid、2- amino -3-butenoic acid, 2- ammonia
One of base -5- hexenoic acid.
9. a kind of preparation method of block water-retaining type concrete admixture as described in claim 1, it is characterised in that: described
Complex reducing agent by weight, has following composition:
2- hydroxyl -2- sulfinatoacetic acid zinc: 40-60%；
2- hydroxyl -2- sulfonatoacetic acid zinc: 1-4%；
L-AA: 1-5%；
It is a kind of in sodium dithionite, potassium hyposulfite or zinc dithionite: 15-35%；Sodium carbonate, sodium bicarbonate, carbon
It is a kind of in sour potassium or saleratus: 10-20%.
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