CN109836539A - A kind of polycarboxylic-acid high water reduction slump retaining agent and preparation method thereof and application method - Google Patents
A kind of polycarboxylic-acid high water reduction slump retaining agent and preparation method thereof and application method Download PDFInfo
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Abstract
The invention discloses a kind of polycarboxylic-acid high water reduction slump retaining agents and preparation method thereof.Specific steps are as follows: (1) isobutene alcohol polyoxyethylene ether is mixed 30 minutes with pure water melts polyoxyethylene ether thoroughly, (2) hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes, (3) by unsaturated acids, hydroxy-ethyl acrylate, water, which is mixed, is used as A liquid, (4) by vitamin C, mercaptopropionic acid, water stirring is used as B liquid, (4) then to isobutene alcohol polyoxyethylene ether, pure water, A liquid and B liquid is added dropwise in dioxygen water mixed liquid simultaneously, (5) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, sodium hydroxide and water adjusting pH and solid content is then added, polycarboxylic acid series high-performance slump retaining agent is made after stirring 20-30 minutes.Loss of concrete during long-distance transportation is solved the problems, such as in use process of the present invention to ensure that the operability of concrete, is worth of widely use.
Description
Technical field
The present invention relates to a kind of polycarboxylic-acid high water reduction slump retaining agents and preparation method thereof, and it is additional to belong to construction material concrete
Agent field.
Background technique
With the development of the building trades such as traffic, water power, municipal administration, high span bridge, floor up to a hundred mansion and petroleum drilling
The engineering constructions such as well platform, seadrome, marine city, seabed tunnel are gradually risen, to concrete performance, intensity index and
Life requirement is higher and higher, and almost all is needed using pump concrete.Pump concrete needs long-distance transportation and higher
It constructs under temperature condition, unavoidably will cause the slump-loss of fresh concrete.For slump-loss it is too fast this
In problem, additive worker usually subtracts so that the retarder such as polycarboxylic acids dehydragent and sodium gluconate, sucrose are compound to improve
The guarantor of aqua is collapsed ability.And add carbohydrate etc. as slow setting ingredient and solve the too fast traditional method of concrete slump loss,
It is far from satisfying requirement of engineering, particularly problematic especially when transportation range is longer, the addition of retarder can not
It fundamentally solves to protect the weak disadvantage of ability of collapsing, excessive retarder volume can be such that the setting time of concrete extends instead, drop
Low concrete quality, influences construction speed.Therefore, exploitation can satisfy a variety of materials use, and protect effect of collapsing, workability and quick
The all preferable slump retaining agent of perception, has a very important significance.
Summary of the invention
The present invention is intended to provide a kind of polycarboxylic-acid high water reduction slump retaining agent, energy-saving production technology lowers consumption and can guarantee excellent
Function of slump protection, water-reducing rate is added in concrete can achieve 30% or more, and the slump keeps 3h to be basically unchanged, while improve mixed
Solidifying each 20% or more the age compressive strength rate of soil, comprehensive service performance are excellent.
Polycarboxylic-acid high water reduction slump retaining agent provided by the invention, preparation method are room temperature preparation, and preparation method is simple, reaction peace
Entirely, polycarboxylic-acid high water reduction slump retaining agent is prepared by room temperature combined oxidation-reduction initiating system, passes through the preparation method research institute
The even molecular weight distribution of the slump retaining agent obtained, performance are stablized, and operating performance is strong in use process, are worth of widely use.
The present invention provides a kind of polycarboxylic-acid high water reduction slump retaining agent, the polycarboxylic-acid high water reduction slump retaining agent is by following original
Material is prepared:
Isobutene alcohol polyoxyethylene ether: 170~200 parts by weight；
Hydrogen peroxide: 1.5~3 parts by weight；
Hydroxy-ethyl acrylate: 16~20 parts by weight；
Unsaturated acids: 10~25 parts by weight；
Vitamin C: 0.5~1 parts by weight；
Mercaptopropionic acid: 0.8~1.8 parts by weight；
Sodium hydroxide: 2.5~4 parts by weight；
Pure water: 320~355 parts by weight.
Further, the unsaturated acids includes one of acrylic acid, methacrylic acid, itaconic acid.
Further, the polycarboxylic-acid high water reduction slump retaining agent is prepared from the following materials:
Isobutene alcohol polyoxyethylene ether: 170 parts by weight；
Hydrogen peroxide: 1.5 parts by weight；
Hydroxy-ethyl acrylate: 16.5 parts by weight；
Acrylic acid: 10 parts by weight；
Vitamin C: 0.5 parts by weight；
Mercaptopropionic acid: 0.8 parts by weight；
Sodium hydroxide: 2.5 parts by weight；
Pure water: 320 parts by weight.
Further, the mass concentration of the hydrogen peroxide is 27.5%.
The present invention provides the preparation methods of above-mentioned polycarboxylic-acid high water reduction slump retaining agent, comprising the following steps:
(1) 170~200 parts by weight of isobutylene alcohol polyoxyethylene ether and 225~235 parts by weight pure water are mixed 30 minutes
Melt isobutene alcohol polyoxyethylene ether thoroughly；
(2) 1.5~3 parts by weight hydrogen peroxide are added in the monomer isobutene alcohol polyoxyethylene ether being stirred and continue stirring 5
Minute；
(3) 10~25 parts by weight unsaturated acids, 16~20 parts by weight of acrylic acid hydroxyl ethyl esters, 25~35 parts by weight pure water are mixed
Stirring is used as A liquid；
(4) 0.5~1 part by weight of vitamin C, 0.8~1.8 parts by weight mercaptopropionic acid, the stirring of 50~55 parts by weight pure water are made
For B liquid；
(5) A liquid and B liquid is then added dropwise simultaneously into mixed liquor obtained by step (2), A liquid time for adding is 1.9-2.1 hours, B liquid
Be added dropwise is 2.4-2.6 hours；
(6) 1 hour being kept the temperature at 20-25 DEG C after A liquid and B liquid are added dropwise, 2.5~4 parts by weight of sodium hydroxide and 20 are then added
~30 parts by weight pure water adjust pH and solid content, and polycarboxylic acid series high-performance slump retaining agent is made after stirring 20-30 minutes.
Above-mentioned preparation method, in step (6), adjusting pH is 6~8.
Above-mentioned preparation method, in step (6), adjusting solid content is 35~45%.
First isobutene alcohol polyoxyethylene ether and pure water are sufficiently stirred in the synthesis process by the present invention, ensure that poly-
Ether monomer is sufficiently dissolved as getting ready with the synthesis of other ingredients below；In second step, hydrogen peroxide and list is first added in we again
Body is sufficiently dissolved, and is also body while being ready for polymerization also for making reaction system become oxidation system in advance
It is the preparation that temperature has premise, the unsaturated acids that we use during the reaction is acrylic acid, methacrylic acid, itaconic acid
One of, these three unsaturated acids can be stablized in the reaction system with isobutene alcohol polyoxyethylene ether to be grafted, and product is promoted
Molecular weight and product function of slump protection.
Above-mentioned preparation method, the performance of obtained slump retaining agent: the slump through when keep 3h it is constant, compression strength data
20% or more is promoted to polycarboxylate high performance water-reducing agent compressive strength rate in ring ratio GB8076-2008 " concrete admixture ", is subtracted
30% or more water rate.The present invention passes through the dosage and ratio for adjusting redox initiator, to adjust the molecular size range of slump retaining agent
With backbone length, making the slump retaining agent being synthesized when in use has better operability.
The present invention provides the application methods of above-mentioned polycarboxylic-acid high water reduction slump retaining agent, it is characterised in that: engineering is practical to be made
With in the process, first designed concrete a variety of materials are added in horizontal mixer after stirring 60 seconds, are gelling material by dosage
The polycarboxylic-acid high water reduction slump retaining agent of the 1-1.5% of material is added thereto, then is stirred and 30 seconds and then is taken the dish out of the pot, carry out the slump and
Compressive strength test.
Beneficial effects of the present invention:
(1) simple process, raw materials are easy to get, and cost is relatively low, it is easy to accomplish industrialized production；
(2) raw material and production process no pollution to the environment；
(3) product properties are more excellent compared with similar products；
(4) polycarboxylic-acid high water reduction slump retaining agent of the present invention, collection high water reduction and high-thin arch dam and one are used, can be used alone, it is raw
Production process is simple and energy-saving, solves the problems, such as loss of concrete during long-distance transportation in use process to protect
The operability for having demonstrate,proved concrete, is worth of widely use.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1
The present embodiment chooses following raw material:
170g isobutene alcohol polyoxyethylene ether, 320g pure water, 1.5g hydrogen peroxide, 10g acrylic acid, 16g hydroxy-ethyl acrylate,
0.5g vitamin C, 0.8g mercaptopropionic acid, 2.5g sodium hydroxide.
Step are as follows:
(1) 170g isobutene alcohol polyoxyethylene ether and 225g pure water are mixed 30 minutes makes isobutene alcohol polyoxyethylene ether
Thoroughly melt;
(2) 1.5g hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes;
(3) 10g acrylic acid, 16g hydroxy-ethyl acrylate, 25g pure water are mixed and are used as A liquid;
(4) 0.5g vitamin C, 0.8g mercaptopropionic acid, the stirring of 50g pure water are regard as B liquid;
(5) A liquid and B liquid then is added dropwise simultaneously into isobutene alcohol polyoxyethylene ether, pure water, dioxygen water mixed liquid, A drop adds
Time is 2 hours, and B drop adds as 2.5 hours;
(6) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, 2.5g sodium hydroxide and 20g pure water adjusting pH to 6- is then added
7 and solid content be 40%, obtained polycarboxylic acid series high-performance slump retaining agent after stirring 20-30 minute.
Embodiment 2
The present embodiment chooses following raw material:
200g isobutene alcohol polyoxyethylene ether, 345g pure water, 3g hydrogen peroxide, 25g methacrylic acid, 20g hydroxy-ethyl acrylate,
1g vitamin C, 1.8g mercaptopropionic acid, 4g sodium hydroxide.
Step are as follows:
(1) 200g isobutene alcohol polyoxyethylene ether and 235g pure water are mixed 30 minutes makes isobutene alcohol polyoxyethylene ether
Thoroughly melt;
(2) 3g hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes;
(3) 25g methacrylic acid, 20g hydroxy-ethyl acrylate, 35g pure water are mixed and are used as A liquid;
(4) 1g vitamin C, 1.8g mercaptopropionic acid, the stirring of 55g pure water are regard as B liquid;
(5) A liquid and B liquid then is added dropwise simultaneously into isobutene alcohol polyoxyethylene ether, pure water, dioxygen water mixed liquid, A drop adds
Time is 2 hours, and B drop adds as 2.5 hours;
(6) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, 4g sodium hydroxide and 20g pure water adjusting pH to 6-7 is then added
And solid content is 40%, and polycarboxylic acid series high-performance slump retaining agent is made after stirring 20-30 minutes.
Embodiment 3
The present embodiment chooses following raw material:
175g isobutene alcohol polyoxyethylene ether, 333g pure water, 2.5g hydrogen peroxide, 20g itaconic acid, 18g hydroxy-ethyl acrylate,
0.8g vitamin C, 1g mercaptopropionic acid, 3g sodium hydroxide.
Step are as follows:
(1) 175g isobutene alcohol polyoxyethylene ether and 230g pure water are mixed 30 minutes makes isobutene alcohol polyoxyethylene ether
Thoroughly melt;
(2) 2.5g hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes;
(3) 20g itaconic acid, 18g hydroxy-ethyl acrylate, 30g pure water are mixed and are used as A liquid;
(4) 0.8g vitamin C, 1g mercaptopropionic acid, the stirring of 53g pure water are regard as B liquid;
(5) A liquid and B liquid then is added dropwise simultaneously into isobutene alcohol polyoxyethylene ether, pure water, dioxygen water mixed liquid, A drop adds
Time is 2 hours, and B drop adds as 2.5 hours;
(6) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, 3g sodium hydroxide and 20g pure water adjusting pH to 6-7 is then added
And solid content is 40%, and polycarboxylic acid series high-performance slump retaining agent is made after stirring 20-30 minutes.
Embodiment 4
The present embodiment chooses following raw material:
185g isobutene alcohol polyoxyethylene ether, 337g pure water, 2.4g hydrogen peroxide, 23g methacrylic acid, 20g acrylic acid hydroxyl second
Ester, 0.6g vitamin C, 1.5g mercaptopropionic acid, 3.5g sodium hydroxide.
Step are as follows:
(1) 185g isobutene alcohol polyoxyethylene ether and 232g pure water are mixed 30 minutes makes isobutene alcohol polyoxyethylene ether
Thoroughly melt;
(2) 2.4g hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes;
(3) 23g methacrylic acid, 20g hydroxy-ethyl acrylate, 32g pure water are mixed and are used as A liquid;
(4) 0.6g vitamin C, 1.5g mercaptopropionic acid, the stirring of 50g pure water are regard as B liquid;
(5) A liquid and B liquid then is added dropwise simultaneously into isobutene alcohol polyoxyethylene ether, pure water, dioxygen water mixed liquid, A drop adds
Time is 2 hours, and B drop adds as 2.5 hours;
(6) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, 3.5g sodium hydroxide and 23g pure water adjusting pH to 6- is then added
7 and solid content be 40%, obtained polycarboxylic acid series high-performance slump retaining agent after stirring 20-30 minute.
Embodiment 5
The present embodiment chooses following raw material:
180g isobutene alcohol polyoxyethylene ether, 335g pure water, 2.2g hydrogen peroxide, 21g itaconic acid, 18g hydroxy-ethyl acrylate,
0.7g vitamin C, 1.3g mercaptopropionic acid, 3g sodium hydroxide.
Step are as follows:
(1) 180g isobutene alcohol polyoxyethylene ether and 230g pure water are mixed 30 minutes makes isobutene alcohol polyoxyethylene ether
Thoroughly melt;
(2) 2.2g hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes;
(3) 21g itaconic acid, 18g hydroxy-ethyl acrylate, 30g pure water are mixed and are used as A liquid;
(4) 0.7g vitamin C, 1.3g mercaptopropionic acid, the stirring of 51g pure water are regard as B liquid;
(5) A liquid and B liquid then is added dropwise simultaneously into isobutene alcohol polyoxyethylene ether, pure water, dioxygen water mixed liquid, A drop adds
Time is 2 hours, and B drop adds as 2.5 hours;
(6) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, 3g sodium hydroxide and 24g pure water adjusting pH to 6-7 is then added
And solid content is 40%, and polycarboxylic acid series high-performance slump retaining agent is made after stirring 20-30 minutes.
Embodiment 6
The present embodiment chooses following raw material:
183g isobutene alcohol polyoxyethylene ether, 335g pure water, 2.1g hydrogen peroxide, 22g itaconic acid, 17g hydroxy-ethyl acrylate,
0.6g vitamin C, 1.5g mercaptopropionic acid, 3.5g sodium hydroxide.
Step are as follows:
(1) 183g isobutene alcohol polyoxyethylene ether and 230g pure water are mixed 30 minutes makes isobutene alcohol polyoxyethylene ether
Thoroughly melt;
(2) 2.1g hydrogen peroxide is added in the monomer being stirred and continues stirring 5 minutes;
(3) 22g itaconic acid, 17g hydroxy-ethyl acrylate, 30g pure water are mixed and are used as A liquid;
(4) 0.6g vitamin C, 1.5g mercaptopropionic acid, the stirring of 51g pure water are regard as B liquid;
(5) A liquid and B liquid then is added dropwise simultaneously into isobutene alcohol polyoxyethylene ether, pure water, dioxygen water mixed liquid, A drop adds
Time is 2 hours, and B drop adds as 2.5 hours;
(6) 1 hour being kept the temperature after A liquid and B liquid are added dropwise, 3.5g sodium hydroxide and 24g pure water adjusting pH to 6- is then added
7 and solid content be 40%, obtained polycarboxylic acid series high-performance slump retaining agent after stirring 20-30 minute.
Slump retaining agent made from Examples 1 to 6 is detected T8076~2008 GB according to national standards.
Application examples 1
By slump retaining agent made from Examples 1 to 6 and presently commercially available tri- kinds of polycarboxylic acid series high-performance slump retaining agents of slump retaining agent number A-C
It is divided into nine groups and carries out cement paste test respectively.
Every group of test raw material is that (reference cement is according to GB8076-2008 appendix A " concrete admixture performance for benchmark cement
Examine and use reference cement technical conditions " require control quality) 500g, water 145g, polycarboxylic acid series high-performance slump retaining agent mother liquor contains admittedly
Amount is 40%, and volume 0.26%, test result is shown in Table 1.
Table 1
The slump retaining agent made from the embodiment of the present invention 1~6 it can be seen from 1 test data of table, 0h to 2h paste flowing degree always
Increasing, in 3h, paste flowing degree is still maintained at initial flow degree or more.Sample A test paste flowing degree is subtracting always
Few, sample B and sample C increased in 1h but then just reduce again always, have for the retentivity of flowing degree of net paste of cement
Certain limitation.
Application examples 2
By slump retaining agent made from Examples 1 to 6 and presently commercially available tri- kinds of polycarboxylic acid series high-performance slump retaining agents of slump retaining agent number A-C
It is divided into nine groups and carries out concrete test respectively.
Note:
Cement: reference cement is according to GB8076-2008 appendix A " concrete admixture service check reference cement technical conditions "
It is required that control quality.
Sand: meet the middle sand that IIth area requires in GB/T14684, but fineness modulus is 2.6 ~ 2.9, clay content is less than 1%.
Stone: meeting GB/T14685, and using graduation two, wherein 5mm ~ 10mm accounts for 40%, 10mm ~ 20mm and accounts for 60%.
Concrete mix: one cube of concrete cement 360kg, sand 819kg, cobble-stone diameter are as follows: 5mm-10mm
400kg, partial size are as follows: 10mm-20mm 601kg, water 220kg, polycarboxylic acid series high-performance slump retaining agent 3.6kg volume are 1%.
Table 2
1 ~ 6 slump 1h ongoing change of embodiment is less than GB8076-2008 " coagulation between 25mm-35mm as can be seen from Table 2
Native additive " in high-performance water reducing agent (retardation setting type) require 60mm and also the embodiment 1-6 slump can keep 2h-3h it
Between be basically unchanged, for practical engineering application have good impetus.1d, 3d, 7d and 28d pressure resistance in embodiment 1-6
Degree is in 205Mpa-220Mpa range inner ring ratio GB8076-2008 " concrete admixture " to high-performance water reducing agent (early-strength)
Middle compression strength data (1d >=180,3d >=170,7d >=145 and 28d >=130) promote 20% or more, diminishing in embodiment 1-6
Rate is also fully met in GB8076-2008 " concrete admixture " to high-performance water reducing agent 30% or more greater than water-reducing rate requirement
Water-reducing rate >=25% requirement.Although commercially available slump retaining agent A ~ C also has certain water-reducing rate, they are much smaller than 25%, in reality
The use that must arrange in pairs or groups with polycarboxylate water-reducer in the application process of border can be only achieved application requirement, although slump 1h ongoing change exists
Within GB8076-2008 " concrete admixture " standard requirements but the slump-retaining difference after 2h, 3h.
Claims (8)
1. a kind of polycarboxylic-acid high water reduction slump retaining agent, it is characterised in that: the polycarboxylic-acid high water reduction slump retaining agent is by following raw material
It is prepared:
Isobutene alcohol polyoxyethylene ether: 170~200 parts by weight；
Hydrogen peroxide: 1.5~3 parts by weight；
Hydroxy-ethyl acrylate: 16~20 parts by weight；
Unsaturated acids: 10~25 parts by weight；
Vitamin C: 0.5~1 parts by weight；
Mercaptopropionic acid: 0.8~1.8 parts by weight；
Sodium hydroxide: 2.5~4 parts by weight；
Pure water: 320~355 parts by weight.
2. polycarboxylic-acid high water reduction slump retaining agent according to claim 1, it is characterised in that: the unsaturated acids includes propylene
One of acid, methacrylic acid, itaconic acid.
3. polycarboxylic-acid high water reduction slump retaining agent according to claim 1, it is characterised in that: the quality of the hydrogen peroxide is dense
Degree is 27.5%.
4. a kind of preparation method of the described in any item polycarboxylic-acid high water reduction slump retaining agents of claim 1 ~ 3, it is characterised in that: packet
Include following steps:
(1) 170~200 parts by weight of isobutylene alcohol polyoxyethylene ether and 225~235 parts by weight pure water are mixed 30 minutes
Melt isobutene alcohol polyoxyethylene ether thoroughly；
(2) 1.5~3 parts by weight hydrogen peroxide are added in the monomer isobutene alcohol polyoxyethylene ether being stirred and continue stirring 5
Minute；
(3) 10~25 parts by weight unsaturated acids, 16~20 parts by weight of acrylic acid hydroxyl ethyl esters, 25~35 parts by weight pure water are mixed
Stirring is used as A liquid；
(4) 0.5~1 part by weight of vitamin C, 0.8~1.8 parts by weight mercaptopropionic acid, the stirring of 50~55 parts by weight pure water are made
For B liquid；
(5) A liquid and B liquid is then added dropwise simultaneously into mixed liquor obtained by step (2), A liquid time for adding is 1.9-2.1 hours, B liquid
Be added dropwise is 2.4-2.6 hours；
(6) 1 hour being kept the temperature at 20-25 DEG C after A liquid and B liquid are added dropwise, 2.5~4 parts by weight of sodium hydroxide and 20 are then added
~30 parts by weight pure water adjust pH and solid content, and polycarboxylic acid series high-performance slump retaining agent is made after stirring 20-30 minutes.
5. the preparation method of polycarboxylic-acid high water reduction slump retaining agent according to claim 4, it is characterised in that: in step (6),
Adjusting pH is 6~8.
6. the preparation method of polycarboxylic-acid high water reduction slump retaining agent according to claim 4, it is characterised in that: in step (6),
Adjusting solid content is 35~45%.
7. the preparation method of polycarboxylic-acid high water reduction slump retaining agent according to claim 4, it is characterised in that: obtained guarantor
Collapse the performance of agent: the slump through when keep 3h constant, it is right in compression strength data ring ratio GB8076-2008 " concrete admixture "
Polycarboxylate high performance water-reducing agent compressive strength rate promotes 20% or more, 30% or more water-reducing rate.
8. a kind of application method of the described in any item polycarboxylic-acid high water reduction slump retaining agents of claim 1 ~ 3, it is characterised in that:
Engineering in actual use, first designed concrete a variety of materials is added in horizontal mixer after stirring 60 seconds,
The polycarboxylic-acid high water reduction slump retaining agent for the 1-1.5% that dosage is cementitious material is added thereto, then is stirred 30 seconds then to go out
Pot carries out the slump and compressive strength test.
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| CN106279557A (en) * | 2015-06-02 | 2017-01-04 | 石家庄市海森化工有限公司 | A kind of energy saving and environment friendly polycarboxylate water-reducer and preparation method thereof |
| CN107652401A (en) * | 2017-09-21 | 2018-02-02 | 攀枝花市吉源科技有限责任公司 | A kind of poly-carboxylic high-performance slump retaining agent and preparation method thereof |
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2019
- 2019-01-28 CN CN201910077919.3A patent/CN109836539A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106279557A (en) * | 2015-06-02 | 2017-01-04 | 石家庄市海森化工有限公司 | A kind of energy saving and environment friendly polycarboxylate water-reducer and preparation method thereof |
| CN106146749A (en) * | 2016-06-27 | 2016-11-23 | 中建商品混凝土西安有限公司 | Meet polycarboxylate water-reducer of 620 meters of super high pump-conveying self-compacting concretes requirements and preparation method thereof |
| CN107652401A (en) * | 2017-09-21 | 2018-02-02 | 攀枝花市吉源科技有限责任公司 | A kind of poly-carboxylic high-performance slump retaining agent and preparation method thereof |
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Application publication date: 20190604 |