CN103396033B - Aliphatic efficient water reducer and preparation method thereof - Google Patents
Aliphatic efficient water reducer and preparation method thereof Download PDFInfo
- Publication number
- CN103396033B CN103396033B CN201310336392.4A CN201310336392A CN103396033B CN 103396033 B CN103396033 B CN 103396033B CN 201310336392 A CN201310336392 A CN 201310336392A CN 103396033 B CN103396033 B CN 103396033B
- Authority
- CN
- China
- Prior art keywords
- aldehyde compound
- reducing agent
- water reducing
- sodium
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a preparation method for an aliphatic efficient water reducer. The preparation method comprises: adding water, a sulfite and an alkaline conditioning agent into a reaction vessel, stirring and heating; at 35-50 DEG C, adding a first portion of an aldehyde compound into the solution, after dropwise adding the aldehyde compound, keeping warm at 50 DEG C for 10-20 min; at 45-50 DEG C, adding a ketone compound into the solution, after dropwise adding the ketone compound, directly adding a second portion of the aldehyde compound, keeping warm at 50-60 DEG C for 20-60 min; at 55-60 DEG C, adding a third portion of the aldehyde compound into the solution, controlling dropwise adding speed on the aldehyde compound to control temperature raise, raising the temperature of the solution gradually to 95 DEG C, after dropwise adding the aldehyde compound, keeping warm at 95-100 DEG C for 1-3 h; and cooling to obtain the liquid water reducer. The prepared aliphatic efficient water reducer is high in water-reducing rate and low in slump loss.
Description
Technical field
The present invention relates to a kind of aliphatic high-efficiency water reducing agent and preparation method, belong to building material technical field.
Background technology
High performance water reducing agent of polyocarboxy acid has the advantages such as high water reducing rate, good slump retaining and environment friendly, is the first-selected water reducer of preparation high performance concrete.Its defect is: polycarboxylate water-reducer price is high, and more responsive to aggregates such as sandstones.Therefore, in the area that aggregate is poor, be still based on high efficiency water reducing agents such as naphthalene system, sulfamate, aliphatics and modified lignin resins.
Aliphatic water reducing agent with acetone, formaldehyde, sulphite etc. for main raw material, through oversulfonate, condensation and obtained anionic polymer tensio-active agent.Aliphatic water reducing agent has that volume is low, sodium sulphate content is few (being less than 1%), winter nodeless mesh, to features such as reinforcing bar non-corrodings, belong to early strong non-air-entraining water-reducing agent, but function of slump protection and adaptability poor.
For solving aliphatic water reducing agent function of slump protection and Adaptive Technology problem, in prior art, usually to collapse ability with the composite guarantor improving water reducer of the retardant such as Sunmorl N 60S or sucrose.But fundamentally can not solve the adding of retardant it and protect the weak shortcoming of ability of collapsing, volume too much can make extend concrete time of coagulation on the contrary, affects construction speed.
Summary of the invention
The object of the present invention is to provide a kind of water-reducing rate is high, Slump Time losing of Large is low aliphatic high-efficiency water reducing agent and preparation method.
For reaching above-mentioned purpose, solution of the present invention is:
A kind of aliphatic high-efficiency water reducing agent preparation method, comprises the following steps:
One, add water, sulphite and alkaline conditioner in a kettle., stir and heat up;
Two, under 35 ~ 50 DEG C of conditions, in solution, add first part of aldehyde compound, after dripping aldehyde compound, make solution be incubated 10 ~ 20 minutes under 50 DEG C of environment;
Three, under 45 ~ 50 DEG C of conditions, in solution, add ketone compounds, after dripping ketone compounds, directly add second part of aldehyde compound, make solution be incubated 20 ~ 60 minutes under 50 ~ 60 DEG C of environment;
Four, under 55 ~ 60 DEG C of conditions, in solution, drip the 3rd part of aldehyde compound, control temperature rise by the rate of addition controlling aldehyde compound, make solution temperature rise to 95 DEG C gradually, after dripping aldehyde compound, make solution be incubated 1 ~ 3 hour under 95 ~ 100 DEG C of environment;
Five, above-mentioned mixing solutions cooling is obtained liquid water reducer.
Further, sulphite is the one in V-Brite B, S-WAT, sodium bisulfite, Sodium Pyrosulfite.
Further, ketone compounds is acetone, butanone, the one in pimelinketone, methylethylketone or methyl phenyl ketone.
Further, first part of aldehyde compound, second part of aldehyde compound and the 3rd part of aldehyde compound are the mixture of the one or both in formaldehyde, paraformaldehyde.
Further, alkaline conditioner is the mixture of one or more (containing two kinds) in sodium hydroxide, potassium hydroxide, sodium phosphate, trisodium phosphate, two sodium polyphosphates, tripoly phosphate sodium STPP, sodium polyphosphate, water glass.
The aliphatic high-efficiency water reducing agent prepared by aforesaid method, is made up of by weight percentage following component: sulphite 8% ~ 15%; Alkaline conditioner 0% ~ 9%; Ketone compounds 8% ~ 12%; Aldehyde compound 21% ~ 39%; All the other are water.
After adopting such scheme, a kind of aliphatic high-efficiency water reducing agent preparation method of the present invention, mainly utilize the condensation reaction of aldehyde ketone under base catalysis and sulfomethylation is carried out to the α position of its carboxyl and introduce sulfonic group to control its molecular weight and water-soluble, its condenses and sulfonation degree is controlled by the ratio of adjustment aldehyde ketone and sulphonating agent, and control its molecular chain structure by the dropping mode adjusting aldehyde compound, obtain comb copolymer, thus obtain the aliphatic high-efficiency water reducing agent with high water-reducing effect and high-thin arch dam performance.Therefore, compared with prior art, a kind of aliphatic high-efficiency water reducing agent preparation method of the present invention has the following advantages:
One, do not need external heat source in production, rely on id reaction heat that reaction solution can be made to reach temperature required, effectively reduce energy consumption and production cost.
Two, produce total duration 4 ~ 5 hours, the reaction times obviously shortens, and saves production cost further.
Three, production technique is simple, and by adjustment raw material ratio and order of addition(of ingredients), each elementary reaction is easy to control, and required equipment is conventional equipment, is convenient to produce.
Four, without the three wastes (waste water,waste gas and industrial residue) discharge in preparation process, environmentally safe.
Meanwhile, the aliphatic high-efficiency water reducing agent prepared by aforesaid method, water-reducing rate is high, and Slump Time losing of Large is low.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment one
A kind of aliphatic high-efficiency water reducing agent preparation method, comprises the following steps: by mass parts, in reactor, adds in four-hole bottle, add 40 parts of sodium hydroxide solution adjust pHs to 12, constant temperature to 40 DEG C by 55 parts of Sodium Pyrosulfites and 250 parts of water.Add about 10 parts of formaldehyde, be warming up to 50 DEG C, be incubated 15 minutes.Add 60 parts of acetone and 20 parts of formaldehyde, temperature controls at 55 DEG C, is incubated 30 minutes.Instill 120 parts of formaldehyde again after insulation terminates, within 1.5 hours, drip off, temperature is warmed up to 95 DEG C from 55 DEG C, 95 DEG C of constant temperature 2 hours after formaldehyde drips, namely obtains product to room temperature after cooling.
The aliphatic high-efficiency water reducing agent prepared by aforesaid method, is made up of by weight percentage following component: Sodium Pyrosulfite 9.9%; Sodium hydroxide solution 7.2%; Acetone 10.8%; Formaldehyde 27.3%; All the other are water.
Embodiment two
A kind of aliphatic high-efficiency water reducing agent preparation method, comprises the following steps: by mass parts, in reactor, adds in four-hole bottle, add 42 parts of potassium hydroxide solution adjust pHs to 12, constant temperature to 35 DEG C by 60 parts of Sodium Pyrosulfites and 240 parts of water.Add about 10 parts of formaldehyde, be warming up to 45 DEG C, be incubated 20 minutes.Add 55 parts of butanone and 20 parts of formaldehyde, temperature controls at 55 DEG C, is incubated 30 minutes.Instill 130 parts of formaldehyde again after insulation terminates, within 1.5 hours, drip off, temperature is warmed up to 95 DEG C from 55 DEG C, 95 DEG C of constant temperature 2 hours after formaldehyde drips, namely obtains product to room temperature after cooling.
The aliphatic high-efficiency water reducing agent prepared by aforesaid method, is made up of by weight percentage following component: Sodium Pyrosulfite 10.8%; Potassium hydroxide solution 7.5%; Butanone 9.9%; Formaldehyde 28.7%; All the other are water.
Embodiment three
A kind of aliphatic high-efficiency water reducing agent preparation method, comprises the following steps: by mass parts, in reactor, adds in four-hole bottle, constant temperature to 35 DEG C by 70 parts of S-WATs and 245 parts of water.Add about 15 parts of formaldehyde, be warming up to 45 DEG C, be incubated 10 minutes.Add 50 parts of acetone and 30 parts of formaldehyde, temperature controls at 55 DEG C, is incubated 30 minutes.Instill 140 parts of formaldehyde again after insulation terminates, within 2 hours, drip off, temperature is warmed up to 95 DEG C from 55 DEG C, 95 DEG C of constant temperature 2 hours after formaldehyde drips, namely obtains product to room temperature after cooling.
The aliphatic high-efficiency water reducing agent prepared by aforesaid method, is made up of by weight percentage following component: S-WAT 12.7%; Acetone 9.1%; Formaldehyde 33.6%; All the other are water.
Embodiment four
A kind of aliphatic high-efficiency water reducing agent preparation method, comprises the following steps: by mass parts, in reactor, adds in four-hole bottle, add 50 parts of sodium hydroxide solution adjust pHs to 13, constant temperature to 45 DEG C by 60 parts of Sodium Pyrosulfites and 260 parts of water.Add about 8 parts of paraformaldehydes, be warming up to 45 DEG C, be incubated 10 minutes.Add 55 parts of butanone and 25 parts of paraformaldehydes, temperature controls at 55 DEG C, is incubated 30 minutes.Instill 130 parts of formaldehyde again after insulation terminates, within 1.5 hours, drip off, temperature is warmed up to 95 DEG C from 55 DEG C, 95 DEG C of constant temperature 2 hours after formaldehyde drips, namely obtains product to room temperature after cooling.
The aliphatic high-efficiency water reducing agent prepared by aforesaid method, is made up of by weight percentage following component: Sodium Pyrosulfite 10.2%; Sodium hydroxide solution 8.5%; Butanone 9.4%; Paraformaldehyde 5.6%; Formaldehyde 22.1%; All the other are water.
High diminishing high-collapse-retentivity aliphatic high-efficiency water reducing agent obtained by embodiment one to embodiment four is tested.
(1) GB 8076-2008 concrete experiments:
Embodiment 1 ~ 4 is synthesized the sample obtained, and commercially available aliphatic high-efficiency water reducing agent A contrasts, adopt reference cement, volume is pressed cement quality 0.45%(and is rolled over solid volume), according to GB 8076-2008 " concrete admixture " standard type high efficiency water reducing agent detection method, survey its concrete water-reducing ratio.Concrete mix is: cement 330kg/m
3, sand 742kg/m
3, stone 1113 kg/m
3(nominal particle diameter is the rubble of 5mm ~ 20mm, and adopt graduation two, wherein 5mm ~ 10mm accounts for 40%, 10mm ~ 20mm and accounts for 60%).Acquired results is as shown in table 1.
Table 1 embodiment performance comparison
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | A |
| Water-reducing rate/% | 24.3 | 23.8 | 22.4 | 24.5 | 19.7 |
(2) C30 concrete experiments:
Embodiment 1 ~ 4 is synthesized the sample obtained, and commercially available aliphatic high-efficiency water reducing agent A contrasts, adopt ordinary Portland cement, river sand, Machine-made Sand, rubble (particle diameter 5 ~ 25mm, continuous size fraction), concrete mix, in table 2, mixes and stirs concrete under the conditions described above, by adjusting the volume of admixture, control initial slump is 220 ± 10mm, and initial extension degree is 580 ± 20mm, measures its slump retention value, divergence retention value, it the results are shown in Table 3.
Table 2 concrete mix
| Cement/kg | Flyash/kg | River sand/kg | Machine-made Sand/kg | Rubble/kg | Water/kg |
| 280 | 60 | 448 | 300 | 1122 | 160 |
Table 3 concrete test result
| Aliphatic water reducing agent | Volume/% | Initial slump (mm) | Initial extension degree (mm) | The 1h slump (mm) | 1h divergence (mm) |
| Embodiment one | 1.65 | 225 | 580 | 220 | 550 |
| Embodiment two | 1.72 | 225 | 570 | 210 | 540 |
| Embodiment three | 1.75 | 220 | 580 | 215 | 530 |
| Embodiment four | 1.68 | 220 | 570 | 225 | 520 |
| A | 2.25 | 230 | 590 | 195 | 340 |
As shown in Table 3, compared with contrast sample A, adopt the water reducer prepared in the embodiment of the present invention compared with reaching identical initial proterties during low-dosage, and 1 hour slump and divergence loss also less, function of slump protection is excellent.Illustrate and adopt the water reducer prepared in the embodiment of the present invention to have higher water-reducing rate and better slump retention ability.
Claims (6)
1. an aliphatic high-efficiency water reducing agent preparation method, is characterized in that: comprise the following steps:
One, add water, sulphite and alkaline conditioner in a kettle., stir and heat up;
Two, under 35 ~ 50 DEG C of conditions, in solution, add first part of aldehyde compound, after dripping aldehyde compound, make solution be incubated 10 ~ 20 minutes under 50 DEG C of environment;
Three, under 45 ~ 50 DEG C of conditions, in solution, add ketone compounds, after dripping ketone compounds, directly add second part of aldehyde compound, make solution be incubated 20 ~ 60 minutes under 50 ~ 60 DEG C of environment;
Four, under 55 ~ 60 DEG C of conditions, in solution, drip the 3rd part of aldehyde compound, control temperature rise by the rate of addition controlling aldehyde compound, make solution temperature rise to 95 DEG C gradually, after dripping aldehyde compound, make solution be incubated 1 ~ 3 hour under 95 ~ 100 DEG C of environment;
Five, above-mentioned mixing solutions cooling is obtained liquid water reducer.
2. a kind of aliphatic high-efficiency water reducing agent preparation method as claimed in claim 1, is characterized in that: sulphite is the one in V-Brite B, S-WAT, sodium bisulfite, Sodium Pyrosulfite.
3. a kind of aliphatic high-efficiency water reducing agent preparation method as claimed in claim 1, is characterized in that: ketone compounds is acetone, butanone, the one in pimelinketone, methylethylketone or methyl phenyl ketone.
4. a kind of aliphatic high-efficiency water reducing agent preparation method as claimed in claim 1, is characterized in that: first part of aldehyde compound, second part of aldehyde compound and the 3rd part of aldehyde compound are the mixture of the one or both in formaldehyde, paraformaldehyde.
5. a kind of aliphatic high-efficiency water reducing agent preparation method as claimed in claim 1, is characterized in that: alkaline conditioner is one or more the mixture in sodium hydroxide, potassium hydroxide, sodium phosphate, trisodium phosphate, two sodium polyphosphates, tripoly phosphate sodium STPP, sodium polyphosphate, water glass.
6. as aliphatic high-efficiency water reducing agent prepared by any one of claim 1 to 5 method, be made up of by weight percentage following component: sulphite 8% ~ 15%; Alkaline conditioner 0% ~ 9%; Ketone compounds 8% ~ 12%; Aldehyde compound 21% ~ 39%; All the other are water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310336392.4A CN103396033B (en) | 2013-08-05 | 2013-08-05 | Aliphatic efficient water reducer and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310336392.4A CN103396033B (en) | 2013-08-05 | 2013-08-05 | Aliphatic efficient water reducer and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103396033A CN103396033A (en) | 2013-11-20 |
| CN103396033B true CN103396033B (en) | 2015-04-08 |
Family
ID=49559827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310336392.4A Expired - Fee Related CN103396033B (en) | 2013-08-05 | 2013-08-05 | Aliphatic efficient water reducer and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103396033B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291725B (en) * | 2014-10-10 | 2016-04-06 | 河南科之杰新材料有限公司 | A kind of preparation method of modified aliphatic water reducing agent |
| CN104710587A (en) * | 2014-10-20 | 2015-06-17 | 金陵科技学院 | Preparation method for low-chroma aliphatic superplasticizer |
| CN104478271B (en) * | 2014-12-09 | 2017-05-03 | 重庆建研科之杰新材料有限公司 | Aliphatic water reducer and preparation method thereof |
| CN106396456B (en) * | 2016-08-26 | 2018-07-03 | 河南科之杰新材料有限公司 | A kind of preparation method of aliphatic powder water-reducing agent |
| CN112608057A (en) * | 2020-07-21 | 2021-04-06 | 科之杰新材料集团河南有限公司 | Water reducing agent and preparation method thereof |
| CN112608058B (en) * | 2020-12-03 | 2022-10-21 | 科之杰新材料集团浙江有限公司 | Concrete micro-foaming agent and preparation method thereof |
| CN115286540B (en) * | 2022-07-19 | 2023-06-02 | 北京市建筑工程研究院有限责任公司 | Preparation method of fresh concrete early strength agent and fresh concrete early strength agent |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575186B (en) * | 2009-05-11 | 2012-06-20 | 江苏尼高科技有限公司 | Aliphatic concrete water reducing agent and preparation process thereof |
-
2013
- 2013-08-05 CN CN201310336392.4A patent/CN103396033B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN103396033A (en) | 2013-11-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103396033B (en) | Aliphatic efficient water reducer and preparation method thereof | |
| CN103288410B (en) | Alpha high-strength gypsum based self-leveling material prepared by adopting phosphogypsum and production process thereof | |
| CN106117482B (en) | A kind of modified high-thin arch dam naphthalene water reducer and preparation method thereof | |
| EP2791077B1 (en) | Dry mix formulations containing carboxylated styrene-butadiene redispersible polymer powders and alumina rich containing cements | |
| CN103193415B (en) | Retarded cement grinding aid and preparation method thereof | |
| CN107840927B (en) | Preparation method of polycarboxylate superplasticizer powder for gypsum-based self-leveling mortar | |
| CN103113036B (en) | Modified aliphatic superplasticizer and preparation method thereof | |
| CN105837724B (en) | A kind of preparation method with the aliphatic water reducing agent of polycarboxylic acids water reducing agent compositional | |
| CN104230204B (en) | A kind of preparation method of collapse protection type aliphatic water reducing agent | |
| CN108840608A (en) | A kind of frost-resistant concrete and preparation method thereof | |
| CN104119026A (en) | Concrete composite water reducing agent | |
| CN103965416A (en) | Early-strength polycarboxylate water reducing agent for component and preparation method for early-strength polycarboxylate water reducing agent | |
| CN108383413A (en) | A kind of novel light resistance to compression foam concrete and preparation method thereof | |
| CN107840592A (en) | A kind of concrete self-repair function additive and preparation method thereof | |
| BR112017028359B1 (en) | cement additive and cement composition | |
| CN104371074A (en) | Low-temperature high-concentration polycarboxylate superplasticizer and preparation method thereof | |
| CN111620589A (en) | Cement grouting material additive capable of adapting to various working conditions and improving performance of grouting material and preparation method and application thereof | |
| CN104291729A (en) | Concrete air entraining agent and preparation method thereof | |
| JP6147194B2 (en) | Rapid hardening cement | |
| CN105199066A (en) | Preparation method of modified naphthalene water reducer | |
| CN108546068A (en) | A kind of self-compaction frost thawing resistance concrete and preparation method thereof that quality is high | |
| CN106746880A (en) | A kind of high-performance permeable concrete cementing agent and its application | |
| CN105566505B (en) | A kind of preparation method of starch sulphonic acid ester | |
| CN103865006A (en) | Polycarboxylate superplasticizer with rust prevention function and preparation method thereof | |
| CN103011670A (en) | Early strength quick-setting polycarboxylic acid type water-reducer and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150408 Termination date: 20210805 |