CN108219055A - A kind of long-acting slump retaining agent and preparation method thereof - Google Patents
A kind of long-acting slump retaining agent and preparation method thereof Download PDFInfo
- Publication number
- CN108219055A CN108219055A CN201611187370.6A CN201611187370A CN108219055A CN 108219055 A CN108219055 A CN 108219055A CN 201611187370 A CN201611187370 A CN 201611187370A CN 108219055 A CN108219055 A CN 108219055A
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- China
- Prior art keywords
- retaining agent
- long
- slump retaining
- preparation
- stirring
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Classifications
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts 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
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/308—Slump-loss preventing agents
Abstract
The present invention provides a kind of preparation method of long-acting slump retaining agent, it is characterised in that：Include the following steps, water, the dissolving of ether heating stirring are added in reaction kettle, is passed through nitrogen, sequentially add methylpropene sodium sulfonate, cross ammonium, stirring；Dropwise addition A, B material, is cooled to 50 DEG C ± 2 DEG C after being added dropwise, add in 30% liquid caustic soda and neutralize, and pH value is controlled between 67, continues moisturizing after stirring 15 minutes, closes nitrogen discharging.It is added in concrete using the slump retaining agent that the above method obtains, not only protects time lengthening of collapsing, also effectively enhance the intensity of concrete.
Description
Technical field
The present invention relates to a kind of long-acting slump retaining agents and preparation method thereof.
Background technology
Slump retaining agent is the additive that can keep concrete slump not immediate loss, and slump retaining agent is substantially retarder,
Hydrated cementitious is delayed to condense, has the function that keep the slump.
Slump retaining agent currently on the market, guarantor is collapsed, and effect is poor, and guarantor collapses the time generally at 1-1.5 hours, more than this time
Concrete will start to solidify, and be not easy to long-distance long-time transport, once concrete occurs solidifying meeting in transportational process
It is attached to inside bulk cement carrier, gently then reduces tank car capacity, concrete can not be poured out, and heavy then entire concrete tank is scrapped.
Invention content
First purpose of the present invention is to provide a kind of preparation method of long-acting slump retaining agent, it is therefore an objective to solve the prior art and ask
Topic, provide it is a kind of protect collapse the time it is longer, reduce bleeding, improve concrete strength slump retaining agent preparation method.
Second object of the present invention is to provide a kind of long-acting slump retaining agent obtained using above-mentioned preparation method.
It is of the present invention solve the problems, such as the technical solution adopted is that：
A kind of preparation method of long-acting slump retaining agent, includes the following steps,
S1, adds in water, ether stirring and dissolving in reaction kettle, and temperature of reaction kettle is warming up to 58 DEG C ± 2 DEG C in whipping process.
S2, temperature start to be passed through nitrogen after 58 DEG C of ± 2 DEG C of stabilizations.
S3 is slowly added to methylpropene sodium sulfonate, and ammonium was slowly added to after stirring evenly, stirring.
A, B material is added dropwise in S4；A material are first added dropwise in reaction kettle, A expects at the uniform velocity to add for 1 hour, and B expects at the uniform velocity to add for 30 minutes, drips
30 minutes are kept the temperature after adding；A material is formulated by thioacetic acid and water, B material prepared by strong ethyl ester, acrylic acid, water and
Into.
S5 is cooled to 50 DEG C ± 2 DEG C, adds in 30% liquid caustic soda of concentration and neutralizes, pH value is controlled between 6-7, continues stirring 15
Nitrogen discharging is closed in moisturizing after minute.
Further, ether, methylpropene sodium sulfonate, cross ammonium mass ratio be 100-110:1：0.065-0.07.
Further, the mass ratio of thioacetic acid and water is 2.5-2.9 in A material：300-305.
Further, strong ethyl ester in B material, acrylic acid, water mass ratio be 105-111:40-45:60-65.
Further, A material were prepared using first 15 minutes, to ensure reaction effect, avoided preparing meeting too early or too late
Cause to react insufficient, influence product quality,
Further, B material were prepared using first 15 minutes.Purpose is to ensure reaction effect, avoiding too early or too late
Preparation can cause to react insufficient, and then influence product quality.
A kind of long-acting slump retaining agent, is obtained using above-mentioned preparation method.
Beneficial effects of the present invention：
1. the time for adding that A, B expect in the present invention is shortened compared with prior art, overreaction can be prevented in this way, is subtracted
The probability of impurity is generated less, more generates effective product.
2. the slump retaining agent in the present invention can increase the mobility of concrete, guarantor is collapsed, and the time, can to extend to 2-2.5 small
When meet concrete long-distance transport requirement.
3. slump retaining agent can be so that the wrapping property of concrete be more preferable, with rubble or cobble after being added to concrete in the present invention
Contact it is more abundant, small bleeding is not in grab bottom phenomenon, and solidify after concrete intensity bigger.
Specific embodiment
The present invention is described in further details below in conjunction with specific embodiment.
Embodiment 1
1st, in 5000L reaction kettles add in 1350 kilograms of water, add 1700 kilograms of import ether start stirring make ether
Temperature of reaction kettle is warming up to 58 DEG C ± 2 DEG C in course of dissolution by dissolving, and temperature, which starts to be passed through nitrogen after stablizing, (it is anti-to generate bunching
Should cause reaction it is more abundant) after be slowly added to 17 kilograms of B2 powder (methylpropene sodium sulfonate) continue stirring 5 minutes, then slowly plus
Enter 6.8 kilograms and cross ammonium, reaction kettle is constantly in stirring in entire reaction process.
2nd, A, B material are prepared,
A material are formulated by 2.9 kilograms of import AC (thioacetic acid) and the stirring of 300 kg of water.
B material are formulated by 222 kilograms of A2 liquid (strong ethyl ester), the stirring of 80 kg of water 120 kg of acrylic acid.
To ensure reaction effect, A material and B material are prepared for 15 minutes before dropwise addition, and too early or crossing party causes reaction not filled
Point, influence product quality.
3rd, in two measuring tanks for being drawn into prepared A, B material above reaction kettle by pipeline, first extraction B is expected to counting
Adding 50 kg of water flushing pipes in measuring tank again, A is prevented to be mixed into B material in expecting, A material add 50 kg of water flushing pipes after extracting,
It prevents from remaining.
4th, start that A, B material is added dropwise, A material are first added dropwise, A expects at the uniform velocity to add for 1 hour, and B expects at the uniform velocity to add for 30 minutes, A, B drop
Time error is added to must not exceed ± 5 minutes.If time for adding it is long or it is too short can cause to chemically react insufficient, influence product
Quality.
5th, it is added dropwise after the completion of A, B material, keeps the temperature 30 minutes, temperature is controlled at 60 DEG C ± 2 DEG C.
6th, ON cycle water is cooled to 50 DEG C ± 2 DEG C and adds in 113 kilogram of 30% liquid caustic soda neutralization, pH value control after keeping the temperature 30 minutes
System between 6-7, after continuing stirring 15 minutes moisturizing 100 kilograms (filling up reaction kettle) close nitrogen afterwards and can discharge.
Embodiment 2
1st, in 5000L reaction kettles add in 1350 kilograms of water, add 1785 kilograms of import ether start stirring make ether
Temperature of reaction kettle is warming up to 58 DEG C ± 2 DEG C in course of dissolution by dissolving, and temperature, which starts to be passed through nitrogen after stablizing, (it is anti-to generate bunching
Should cause reaction it is more abundant) after be slowly added to 17 kilograms of B2 powder (methylpropene sodium sulfonate) continue stirring 5 minutes, then slowly plus
Enter 6.5 kilograms and cross ammonium, reaction kettle is constantly in stirring in entire reaction process.
2nd, A, B material are prepared,
A material are formulated by 2.5 kilograms of import AC (thioacetic acid) and the stirring of 300 kg of water.
B material are formulated by 210 kilograms of A2 liquid (strong ethyl ester), the stirring of 80 kg of water 120 kg of acrylic acid.
To ensure reaction effect, A material and B material are prepared for 15 minutes before dropwise addition, and too early or crossing party causes reaction not filled
Point, influence product quality.
3rd, in two measuring tanks for being drawn into prepared A, B material above reaction kettle by pipeline, first extraction B is expected to counting
Adding 50 kg of water flushing pipes in measuring tank again, A is prevented to be mixed into B material in expecting, A material add 50 kg of water flushing pipes after extracting,
It prevents from remaining.
4th, start that A, B material is added dropwise, A material are first added dropwise, A expects at the uniform velocity to add for 1 hour, and B expects at the uniform velocity to add for 30 minutes, A, B drop
Time error is added to must not exceed ± 5 minutes.If time for adding it is long or it is too short can cause to chemically react insufficient, influence product
Quality.
5th, it is added dropwise after the completion of A, B material, keeps the temperature 30 minutes, temperature is controlled at 60 DEG C ± 2 DEG C.
6th, ON cycle water is cooled to 50 DEG C ± 2 DEG C and adds in 113 kilogram of 30% liquid caustic soda neutralization, pH value control after keeping the temperature 30 minutes
Between 6-7, continuing moisturizing closing nitrogen to after filling up reaction kettle after stirring 15 minutes can discharge system.
Embodiment 3
1st, in 5000L reaction kettles add in 1350 kilograms of water, add 1700 kilograms of import ether start stirring make ether
Temperature of reaction kettle is warming up to 58 DEG C ± 2 DEG C in course of dissolution by dissolving, and temperature, which starts to be passed through nitrogen after stablizing, (it is anti-to generate bunching
Should cause reaction it is more abundant) after be slowly added to 17 kilograms of B2 powder (methylpropene sodium sulfonate) continue stirring 5 minutes, then slowly plus
Enter 7 kilograms and cross ammonium, reaction kettle is constantly in stirring in entire reaction process.
2nd, A, B material are prepared,
A material are formulated by 2.9 kilograms of import AC (thioacetic acid) and the stirring of 300 kg of water.
B material are formulated by 222 kilograms of A2 liquid (strong ethyl ester), the stirring of 80 kg of water 120 kg of acrylic acid.
To ensure reaction effect, A material and B material are prepared for 15 minutes before dropwise addition, and too early or crossing party causes reaction not filled
Point, influence product quality.
3rd, in two measuring tanks for being drawn into prepared A, B material above reaction kettle by pipeline, first extraction B is expected to counting
Adding 50 kg of water flushing pipes in measuring tank again, A is prevented to be mixed into B material in expecting, A material add 50 kg of water flushing pipes after extracting,
It prevents from remaining.
4th, start that A, B material is added dropwise, A material are first added dropwise, A expects at the uniform velocity to add for 1 hour, and B expects at the uniform velocity to add for 30 minutes, A, B drop
Time error is added to must not exceed ± 5 minutes.If time for adding it is long or it is too short can cause to chemically react insufficient, influence product
Quality.
5th, it is added dropwise after the completion of A, B material, keeps the temperature 30 minutes, temperature is controlled at 60 DEG C ± 2 DEG C.
6th, ON cycle water is cooled to 50 DEG C ± 2 DEG C and adds in 113 kilogram of 30% liquid caustic soda neutralization, pH value control after keeping the temperature 30 minutes
Between 6-7, continuing moisturizing closing nitrogen to after filling up reaction kettle after stirring 15 minutes can discharge system.
The embodiment of the present invention 1, embodiment 2,3 product of embodiment and prior art slump retaining agent are added separately in concrete
Proceed to contrasting detection, as a result see the table below 1：
Table 1
| Guarantor is collapsed the time (h) | Concrete strength (kPa) | |
| Embodiment 1 | 2.5 | 31 |
| Embodiment 2 | 2.2 | 30 |
| Embodiment 3 | 2.3 | 30 |
| Prior art slump retaining agent | 1.2 | 24 |
From table 1 it follows that the slump retaining agent in the present invention is compared with prior art slump retaining agent, guarantor's time of collapsing is longer,
The effectively intensity of enhancing concrete.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope of present disclosure, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of long-acting slump retaining agent, it is characterised in that：Include the following steps,
S1, adds in water, ether stirring and dissolving in reaction kettle, and temperature of reaction kettle is warming up to 58 DEG C ± 2 DEG C in whipping process；
S2, temperature start to be passed through nitrogen after 58 DEG C of ± 2 DEG C of stabilizations；
S3 is slowly added to methylpropene sodium sulfonate, and ammonium was slowly added to after stirring evenly, stirring；
A, B material is added dropwise in S4；A material are first added dropwise in reaction kettle, A expects at the uniform velocity to add for 1 hour, and B expects at the uniform velocity to add for 30 minutes, drips
30 minutes are kept the temperature after finishing；The A material are formulated by thioacetic acid and water, and B material are formulated by strong ethyl ester, acrylic acid, water；
S5 is cooled to 50 DEG C ± 2 DEG C, adds in 30% liquid caustic soda of concentration and neutralizes, and pH value is controlled between 6-7, continues stirring 15 minutes
Nitrogen discharging is closed in moisturizing afterwards.
2. a kind of preparation method of long-acting slump retaining agent as described in claim 1, it is characterised in that：Ether, metering system sulphur
The mass ratio of sour sodium, excessively ammonium is 100-110:1：0.065-0.07.
3. a kind of preparation method of long-acting slump retaining agent as described in claim 1, it is characterised in that：A material in thioacetic acid with
The mass ratio of water is 2.5-2.9：300-305.
4. a kind of preparation method of long-acting slump retaining agent as described in claim 1, it is characterised in that：Strong ethyl ester, propylene in B material
Sour, water mass ratio is 105-111:40-45:60-65.
5. a kind of preparation method of long-acting slump retaining agent as described in claim 1, it is characterised in that：The A material use preceding 15
Minute is prepared.
6. a kind of preparation method of long-acting slump retaining agent as described in claim 1, it is characterised in that：The B material use preceding 15
Minute is prepared.
7. a kind of long-acting slump retaining agent is obtained using the preparation method as described in claim 1-6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611187370.6A CN108219055A (en) | 2016-12-21 | 2016-12-21 | A kind of long-acting slump retaining agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611187370.6A CN108219055A (en) | 2016-12-21 | 2016-12-21 | A kind of long-acting slump retaining agent and preparation method thereof |
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| CN108219055A true CN108219055A (en) | 2018-06-29 |
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| CN201611187370.6A Pending CN108219055A (en) | 2016-12-21 | 2016-12-21 | A kind of long-acting slump retaining agent and preparation method thereof |
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Citations (5)
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| CN102584092A (en) * | 2012-02-24 | 2012-07-18 | 河北金舵建材科技开发有限公司 | Slump loss resistant slow release polycarboxylic acid water reducer and preparation method thereof |
| CN103724560A (en) * | 2013-12-31 | 2014-04-16 | 大连市铭源全科技开发有限公司 | Super-strong slump retaining agent and processing method thereof |
| CN103833939A (en) * | 2012-11-26 | 2014-06-04 | 科之杰新材料集团有限公司 | Preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retaining agent prepared through method |
| CN104973816A (en) * | 2015-06-25 | 2015-10-14 | 贵州省瓮安新源新材料有限公司 | Polycarboxylic acid slump retaining agent with low bleeding rate and preparation method thereof |
| CN105884979A (en) * | 2016-04-08 | 2016-08-24 | 湖南铭煌科技发展有限公司 | Normal-temperature preparation method of slow-release polycarboxylic acid slump retaining agent |
-
2016
- 2016-12-21 CN CN201611187370.6A patent/CN108219055A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584092A (en) * | 2012-02-24 | 2012-07-18 | 河北金舵建材科技开发有限公司 | Slump loss resistant slow release polycarboxylic acid water reducer and preparation method thereof |
| CN103833939A (en) * | 2012-11-26 | 2014-06-04 | 科之杰新材料集团有限公司 | Preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retaining agent prepared through method |
| CN103724560A (en) * | 2013-12-31 | 2014-04-16 | 大连市铭源全科技开发有限公司 | Super-strong slump retaining agent and processing method thereof |
| CN104973816A (en) * | 2015-06-25 | 2015-10-14 | 贵州省瓮安新源新材料有限公司 | Polycarboxylic acid slump retaining agent with low bleeding rate and preparation method thereof |
| CN105884979A (en) * | 2016-04-08 | 2016-08-24 | 湖南铭煌科技发展有限公司 | Normal-temperature preparation method of slow-release polycarboxylic acid slump retaining agent |
Non-Patent Citations (1)
| Title |
|---|
| 中国建筑学会建材分会混凝土外加剂应用技术专业委员会: "《聚羧酸系高性能减水剂制备、性能与应用技术新进展》", 31 May 2013, 北京理工大学出版社 * |
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Application publication date: 20180629 |