CN106632859A - Preparation method of starch grafting concrete thickener - Google Patents
Preparation method of starch grafting concrete thickener Download PDFInfo
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- CN106632859A CN106632859A CN201611139403.XA CN201611139403A CN106632859A CN 106632859 A CN106632859 A CN 106632859A CN 201611139403 A CN201611139403 A CN 201611139403A CN 106632859 A CN106632859 A CN 106632859A
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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
-
- 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
- C04B24/38—Polysaccharides or derivatives thereof
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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
- C04B2103/44—Thickening, gelling or viscosity increasing agents
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
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- Graft Or Block Polymers (AREA)
Abstract
The invention discloses a preparation method of a starch grafting concrete thickener. The preparation method comprises the following steps: 1) pasting starch and obtaining a starch free radical under the effect of an initiator A; 2) performing water-phase free radical polymerization of the starch free radical, unsaturated amide small monomer and unsaturated sulfonic acid small monomer under the joint effect of an initiator B and a reducing agent system to obtain a copolymerization product; and 3) after reaction, washing with ethanol, performing suction filtration, drying, adjusting the pH to 6-7 with alkali liquor, and adding water to obtain a starch grafting concrete thickener with concentration of 10-20% by mass. The method disclosed by the invention has high efficiency and is easy to operate. The starch grafting concrete thickener prepared in the invention can remarkably improve the water retention capacity of concrete, and solves the problems of disintegration and bleeding of concrete while the product performance is stable.
Description
Technical field
The present invention relates to a kind of preparation method of concrete thickener, and in particular to increase to a kind of Starch graft copolymer coal-water concrete
Thick dose of preparation method, belongs to concrete admixture field.
Background technology
With the continuous progress of society, industrial development requires more and more higher to construction quality.Concrete is used as engineering construction
Middle important materials, its performance has obtained nearly paying attention to.But, during practical engineering application, due to disappearing for buildings and resources
Consumption, aggregate quality is deteriorated on market, causes level with unreasonable, adds in laboratory and engineering to ensure the stream of fresh concrete
Become performance, improve polycarboxylate water-reducer volume, and third generation high performance water reducing agent of polyocarboxy acid is quicker compared with other water reducers to volume
, so that the concrete workability prepared is bad, or even there are the phenomenons such as isolation, bleeding in sense.Isolation, the bleeding of concrete is to it
Performance has extremely serious harm, directly influences the performances such as intensity, weathering resistance and the anti-erosion of concrete, makes construction quality
Cannot be guaranteed.The reason for this problem occur, fundamentally analyzes, and is because that slurry viscosity not enough causes its workability, bag
The property wrapped up in is bad, so as to occur isolation, bleeding the problems such as.
The problems such as in order to improve concrete performance, solution concrete disintegration, bleeding, it is usually added into thickener to increase slurry
Cohesiveness and cohesive force so that ensureing the homogeneity of its performance.
At present engineers and technicians can soluble high molecular polymer such as glycan class, polyvinyl alcohol, xanthans, fiber by addition
Plain ether etc. improves the mix state of concrete as thickener, makes the uniform high-quality of concrete performance, but all there is certain asking
Topic.Glycan class can cause initial set and final setting time to extend with the increase of its volume, and early age strength of concrete is too low.Polyvinyl alcohol
Dissolubility it is poor, be also easy to produce flocculent deposit during with compounding polycarboxylic acid, make additive homogeneity be deteriorated.Xanthans and cellulose ether
On the one hand concrete water bleeding can be effectively reduced, the slump of concrete is made but then to be reduced, working performance of concrete is reduced,
Difficulty of construction is increased.Above-mentioned concrete thickener is all difficult to solve the problems, such as Practical Project.
The content of the invention
The invention aims to improve the deficiencies in the prior art and provide a kind of Starch graft copolymer coal-water concrete thickener
Preparation method, it is highly resistant to concrete disintegration, bleeding having under the premise of good compatibility with water reducer.
The technical scheme is that：. a kind of preparation method of Starch graft copolymer coal-water concrete thickener, its concrete steps is such as
Under：
1) preparation of Starch Free Radicals：Starch is soluble in water, and stirring is configured to mass percent concentration for 15～30%
Starch solution, heat 50～70 DEG C of gelatinizations, addition accounts for the initiator A of starch quality 0.5～1.2%, and 1～2h of reaction is formed sediment
Powder free-atom aqueous solution；
2) it is under the conditions of 35～60 DEG C, unsaturated amides minor comonomer, unsaturated sulfonic acid class minor comonomer, Starch Free Radicals are molten
The oxidation-reduction system of liquid, initiator B and reducing agent composition enters water-filling phase Raolical polymerizable, 2～4h of reaction time；Its
The mass ratio of middle unsaturated amides minor comonomer, unsaturated sulfonic acid class minor comonomer, starch, initiator B and reducing agent is 1:(0.2～
0.8):(1.2-3.3):(0.05～0.15):(0.01～0.06)；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 6～7 with alkali lye adjustment PH, added water and obtain quality percentage
Concentration is 10～20% Starch graft copolymer coal-water concrete thickener.
Preferred steps 1) in starch for tapioca, farina, cornstarch or wheaten starch one kind or two
Plant combination of the above.Preferred steps 1) in initiator A for potassium permanganate, ammonium ceric nitrate or benzoyl peroxide one or two
Combination of the above.
Preferred steps 2) described in unsaturated acyl amine minor comonomer formula：R1CONR2R3Represent, wherein R1For 2～6
The thiazolinyl of carbon atom, R2, R3For the alkyl or H of 1～4 carbon atom.Wherein R1For the thiazolinyl of 2～6 carbon atoms, R2, R3For 1
The alkyl or H of～4 carbon atoms.More preferably step 2) described in unsaturated acyl amine minor comonomer be acrylamide, isopropyl
One or two in acrylamide, NVP, N- vinyl acetamides or N- methyl-Nvinylacetamides
Combination of the above.
Preferred steps 2) in unsaturated sulfonic acid class minor comonomer be to use formula：R4SO3M represents, wherein R4For 3～8 carbon originals
The unsaturated olefin substratess of son, M is H, metal ion, ammonium or organic amino group.More preferably step 2) in unsaturated sulfonic acid class
Minor comonomer is ALS, 2- acrylamide-2-methylpro panesulfonic acids, methyl allyloxy sodium sulfonate, vinyl sulfonic acid
The one or more combination of amine or styrene sulfonic acid potassium.
Preferred steps 2) in initiator B be persulfuric acid thing or peroxide.More preferably step 2) in initiator B be double
One or more combinations of oxygen water, ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate.
Preferred steps 2) in reducing agent for sodium hydrogensulfite, sodium formaldehyde sulfoxylate, sodium ascorbate or arabo-ascorbic acid one kind
Or two or more combinations；Preferred steps 3) in alkali lye be NaOH or potassium hydroxide one or two combinations.
The present invention principle be：Starch degree of grafting is high, belongs to weak covalently bonded carbon carbon heterochain, and structure has multiple hydroxyls
Base, grafting active sites are more, and Starch Free Radicals graft copolymerization is more ripe, can be by radical polymerization in Starch Free Radicals
Upper access unsaturated amides minor comonomer and unsaturated sulfonic acid class minor comonomer.Unsaturated amides minor comonomer reactivity is high, can improve
The molecular weight of graft copolymer, improves thickening properties, meanwhile, amide group has good hydrophily and hydrolysis temperature,
Improve polymeric hydrophilic ability.Sulfonic acid group can be formed by Hydrogenbond with water and combine water in unsaturated sulfonic acid class minor comonomer
Layer, meanwhile, sulfonic acid group charge density is big, and Stability Analysis of Structures so as to insensitive to acid, alkali, salt enhances polymer in cement mortar
Adaptability in body.Starch backbone is long, and sub-chain motion is limited, and stronger sterically hindered ability increases the distance between cement granules,
Hydrone is set easily to enter, while it there are stronger water absorbing properties, there is provided stronger water holding capacity.
Wherein, high polymer main chain can provide system viscosity, so as to improve cement slurry viscosity, improve concrete consistence；
Amide side chain group has good hydrophily, reduces surface tension, reduces the resistance of motion between cement granules；Pendant sulfonic acid base
There is stronger anionic property in group, is adsorbed in cement particle surface, strengthens cementitiousness between particle；Side chain Starch Free Radicals roll into a ball hydroxyl
Base forms hydrogen bond with water, with good hydrophilic performance, while good sterically hindered effect is provided, between appropriate disperse cement particles
Away from making hydrone easily enter.
Beneficial effect：
1. primary raw material starch yield height used by the inventive method, abundance, cheap and easy to get.
2. the Starch graft copolymer coal-water concrete thickener products good water solubility that prepared by the inventive method, it is not stratified during storage, with
Stable homogeneous during polycarboxylic acids water reducing agent compositional, and adaptability is good.
3. the inventive method prepare Starch graft copolymer coal-water concrete thickener products whole preparation process in it is safe and reliable, behaviour
Make step simple and convenient, nontoxic pollution-free, the advantages of environmentally safe.
4. the concrete thickener that prepared by the inventive method ensure that mixed while concrete disintegration, bleeding problem is improved
Coagulate the service behaviour of soil.
Specific embodiment
Technical solution of the present invention is described in further detail below by embodiment.
Embodiment 1
1) tapioca 65g is soluble in water, stirring is configured to the starch solution that mass percent concentration is 25%, plus
69 DEG C of gelatinizations of heat, add 0.51g ammonium ceric nitrates, reaction 1.5h to obtain Starch Free Radicals solution；
2) under the conditions of 36 DEG C, N-isopropylacrylamide 20g, ALS 4g are added in reactor, stirring is equal
It is even, the aqueous solution of the different ascorbic acids of 2.8g containing potassium peroxydisulfate and 0.9g is then added dropwise respectively, reaction time 3h obtains starch-grafted
Thing；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 6 with NaOH adjustment PH, added water and obtain quality percentage
Specific concentration is 15% Starch graft copolymer coal-water concrete thickener.
Embodiment 2
1) cornstarch 25g is soluble in water, stirring is configured to the starch solution that mass percent concentration is 30%, plus
51 DEG C of gelatinizations of heat, add 0.30g potassium permanganate, reaction 1h to obtain Starch Free Radicals solution；
2) under the conditions of 60 DEG C, acrylamide 20g, methyl allyloxy sodium sulfonate 15g are added in reactor, stirring is equal
It is even, the aqueous solution of 1.1g containing ammonium persulfate and 0.21g sodium ascorbates is then added dropwise respectively, reaction time 4h obtains starch and connects
Branch thing；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 6 with NaOH adjustment PH, added water and obtain quality percentage
Specific concentration is 20% Starch graft copolymer coal-water concrete thickener.
Embodiment 3：
1) farina 39g is soluble in water, stirring is configured to the starch solution that mass percent concentration is 15%,
70 DEG C of gelatinizations of heating, add 0.195g benzoyl peroxides, reaction 2h to obtain Starch Free Radicals solution；
2) under the conditions of 46 DEG C, NVP 20g, 2- acrylamide-2-methylpro panesulfonic acid 8g is added
In reactor, stir, the aqueous solution of 2.9g containing hydrogen peroxide and 1.2g sodium hydrogensulfites, reaction time are then added dropwise respectively
2h, obtains Starch graft copolymer coal-water；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 7 with potassium hydroxide adjustment PH, added water and obtain quality percentage
Specific concentration is 10% Starch graft copolymer coal-water concrete thickener.
Embodiment 4：
1) wheaten starch 48g is soluble in water, stirring is configured to the starch solution that mass percent concentration is 17%, plus
58 DEG C of gelatinizations of heat, add 0.43g ammonium ceric nitrates, reaction 1.5h to obtain Starch Free Radicals solution；
2) under the conditions of 60 DEG C, N- vinyl acetamides 20g, vinyl sulfonic acid amine 4g are added in reactor, stirring is equal
It is even, the aqueous solution of the different ascorbic acids of 1.6g containing sodium peroxydisulfate and 0.8g is then added dropwise respectively, reaction time 3.5h obtains starch and connects
Branch thing；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 6 with potassium hydroxide adjustment PH, added water and obtain quality percentage
Specific concentration is 17% Starch graft copolymer coal-water concrete thickener.
Embodiment 5：
1) tapioca 37g is soluble in water, stirring is configured to the starch solution that mass percent concentration is 19%, plus
62 DEG C of gelatinizations of heat, add 0.43g benzoyl peroxides, reaction 2h to obtain Starch Free Radicals solution；
2) under the conditions of 38 DEG C, N- methyl-Nvinylacetamide 20g, styrene sulfonic acid potassium 9g are added in reactor,
Stir, the aqueous solution of 2.1g containing hydrogen peroxide and 0.67g sodium formaldehyde sulfoxylates is then added dropwise respectively, reaction time 4h obtains starch and connects
Branch thing；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 7 with NaOH adjustment PH,.Add water and obtain quality hundred
Divide the Starch graft copolymer coal-water concrete thickener that specific concentration is 13%.
Above example 1 is evaluated to the product of embodiment 5, and selects a kind of commercial concrete thickener methylol fine
Dimension element makees reference.
(1) cement paste performance evaluation
Cement paste is tested according to GB/T8076-2008《Concrete admixture homogeneity experimental technique》Regulation is carried out, base
Quasi- cement 300g, uses water 87g；Cement paste thickening effect detection is carried out to sample by DV-S digital displays viscosimeter, 1 is shown in Table.
The cement paste performance evaluation of table 1
(2) concrete performance evaluation
It is with reference to JGJ55-2011 that concrete performance evaluate it to coordinate when experiment《Design of common concrete proportioning is advised
Journey》Carry out, cement on the basis of cement used, wherein, blank assay group is not added with tackifier, using the experimental group thickening of thickener
Agent volume is the 2% of additive quality, and match ratio is shown in Table 2.With reference to GB8076-2008《Concrete admixture》Sample is mixed
Solidifying soil performance evaluation, is shown in Table 3.
Concrete mix (the kg/m of table 23)
| Cement | Flyash | Breeze | Sand | Stone | Additive | Water |
| 235 | 50 | 55 | 783 | 1052 | 4.2 | 175 |
The concrete performance evaluation of table 3
Claims (10)
1. a kind of preparation method of Starch graft copolymer coal-water concrete thickener, it is comprised the following steps that：
1) preparation of Starch Free Radicals：Starch is soluble in water, and stirring is configured to the shallow lake that mass percent concentration is 15～30%
Powder solution, heats 50～70 DEG C of gelatinizations, and addition accounts for the initiator A of starch quality 0.5～1.2%, and 1～2h of reaction obtains starch certainly
By based sols；
2) under the conditions of 35～60 DEG C, by unsaturated amides minor comonomer, unsaturated sulfonic acid class minor comonomer, Starch Free Radicals solution,
The oxidation-reduction system of initiator B and reducing agent composition enters water-filling phase Raolical polymerizable, 2～4h of reaction time；Wherein not
The mass ratio of saturated amide minor comonomer, unsaturated sulfonic acid class minor comonomer, starch, initiator B and reducing agent is 1:(0.2～0.8):
(1.2-3.3):(0.05～0.15):(0.01～0.06)；
3) washed with ethanol after the completion of reacting, suction filtration, be dried, be 6～7 with alkali lye adjustment PH, added water and obtain mass percentage concentration
For 10～20% Starch graft copolymer coal-water concrete thickener.
2. preparation method according to claim 1, it is characterised in that step 1) described in starch be tapioca, Ma Ling
One or more combinations of sweet potato starch, cornstarch or wheaten starch.
3. preparation method according to claim 1, it is characterised in that step 1) described in initiator A be potassium permanganate,
One or more combinations of ammonium ceric nitrate or benzoyl peroxide.
4. preparation method according to claim 1, it is characterised in that step 2) described in unsaturated acyl amine minor comonomer use
Formula：R1CONR2R3Represent, wherein R1For the thiazolinyl of 2～6 carbon atoms, R2, R3For the alkyl or H of 1～4 carbon atom；Its
Middle R1For the thiazolinyl of 2～6 carbon atoms, R2, R3For the alkyl or H of 1～4 carbon atom.
5. preparation method according to claim 1, it is characterised in that step 2) described in unsaturated acyl amine minor comonomer be
Acrylamide, N-isopropylacrylamide, NVP, N- vinyl acetamides or N- methyl-N-vinyl acetyl
One or more combinations in amine.
6. preparation method according to claim 1, it is characterised in that step 2) described in unsaturated sulfonic acid class minor comonomer
It is to use formula：R4SO3M represents, wherein R4For the unsaturated olefin substratess of 3～8 carbon atoms, M be H, metal ion, ammonium or
Organic amino group.
7. preparation method according to claim 1, it is characterised in that step 2) described in unsaturated sulfonic acid class minor comonomer
For ALS, 2- acrylamide-2-methylpro panesulfonic acids, methyl allyloxy sodium sulfonate, vinyl sulfonic acid amine or benzene
The one or more combination of vinyl sulfonic acid potassium.
8. preparation method according to claim 1, it is characterised in that step 2) described in initiator B be persulfuric acid thing or
Peroxide.
9. preparation method according to claim 1, it is characterised in that step 2) described in initiator B be hydrogen peroxide, mistake
One or more combinations of ammonium sulfate, sodium peroxydisulfate or potassium peroxydisulfate.
10. preparation method according to claim 1, it is characterised in that step 2) described in reducing agent be bisulfite
One or more combinations of sodium, sodium formaldehyde sulfoxylate, sodium ascorbate or arabo-ascorbic acid；Step 3) in alkali lye be NaOH
Or one or two combinations of potassium hydroxide.
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Cited By (9)
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| CN107827399A (en) * | 2017-11-09 | 2018-03-23 | 安徽艾米伦特建材科技有限公司 | Cement mortar and preparation method thereof |
| CN107827387A (en) * | 2017-11-09 | 2018-03-23 | 安徽艾米伦特建材科技有限公司 | Cement mortar water-loss reducer and preparation method thereof |
| CN110563409A (en) * | 2019-10-09 | 2019-12-13 | 中建商品混凝土有限公司 | steam-curing-free light and ultra-high-strength concrete and preparation method thereof |
| CN110963733A (en) * | 2018-09-29 | 2020-04-07 | 镇江苏博特新材料有限公司 | Preparation method of water-based cement hydration rate regulating material |
| CN111943560A (en) * | 2020-08-06 | 2020-11-17 | 武汉源锦建材科技有限公司 | Low-resilience alkali-free liquid accelerator and preparation method thereof |
| CN112661906A (en) * | 2020-12-02 | 2021-04-16 | 广东省科学院化工研究所 | Starch graft polymer and preparation method and application thereof |
| CN112708025A (en) * | 2020-12-28 | 2021-04-27 | 科之杰新材料集团有限公司 | Anti-segregation intermediate, self-compacting concrete anti-segregation agent and preparation method thereof |
| CN114907521A (en) * | 2022-07-04 | 2022-08-16 | 中国水利水电第七工程局有限公司 | Film-forming protection type anti-dispersant for underwater concrete and preparation method thereof |
| CN115893921A (en) * | 2021-09-30 | 2023-04-04 | 中国石油化工股份有限公司 | Underwater undispersed cement slurry for well drilling plugging and preparation method and application thereof |
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|---|---|---|---|---|
| CN107827387A (en) * | 2017-11-09 | 2018-03-23 | 安徽艾米伦特建材科技有限公司 | Cement mortar water-loss reducer and preparation method thereof |
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| CN110963733A (en) * | 2018-09-29 | 2020-04-07 | 镇江苏博特新材料有限公司 | Preparation method of water-based cement hydration rate regulating material |
| CN110563409B (en) * | 2019-10-09 | 2021-11-02 | 中建商品混凝土有限公司 | Steam-curing-free light and ultra-high-strength concrete and preparation method thereof |
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| CN111943560B (en) * | 2020-08-06 | 2022-09-09 | 武汉源锦建材科技有限公司 | Low-resilience alkali-free liquid accelerator and preparation method thereof |
| CN111943560A (en) * | 2020-08-06 | 2020-11-17 | 武汉源锦建材科技有限公司 | Low-resilience alkali-free liquid accelerator and preparation method thereof |
| CN112661906A (en) * | 2020-12-02 | 2021-04-16 | 广东省科学院化工研究所 | Starch graft polymer and preparation method and application thereof |
| CN112708025A (en) * | 2020-12-28 | 2021-04-27 | 科之杰新材料集团有限公司 | Anti-segregation intermediate, self-compacting concrete anti-segregation agent and preparation method thereof |
| CN112708025B (en) * | 2020-12-28 | 2023-08-25 | 科之杰新材料集团有限公司 | Anti-segregation intermediate, self-compacting concrete anti-segregation agent and preparation method thereof |
| CN115893921A (en) * | 2021-09-30 | 2023-04-04 | 中国石油化工股份有限公司 | Underwater undispersed cement slurry for well drilling plugging and preparation method and application thereof |
| CN115893921B (en) * | 2021-09-30 | 2024-06-07 | 中国石油化工股份有限公司 | Underwater non-dispersed cement paste for well drilling plugging and preparation method and application thereof |
| CN114907521A (en) * | 2022-07-04 | 2022-08-16 | 中国水利水电第七工程局有限公司 | Film-forming protection type anti-dispersant for underwater concrete and preparation method thereof |
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