CN107189026A - A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer - Google Patents
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer Download PDFInfo
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- CN107189026A CN107189026A CN201710339643.2A CN201710339643A CN107189026A CN 107189026 A CN107189026 A CN 107189026A CN 201710339643 A CN201710339643 A CN 201710339643A CN 107189026 A CN107189026 A CN 107189026A
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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
- C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
- C08F299/02—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
- C08F299/026—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from the reaction products of polyepoxides and unsaturated monocarboxylic acids, their anhydrides, halogenides or esters with low molecular weight
-
- 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
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
-
- 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
- C04B2103/302—Water reducers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Polyethers (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer of the present invention, first by adding poly glycol monomethyl ether 1000, poly glycol monomethyl ether 2000, methacrylic acid, p-methyl benzenesulfonic acid, hydroquinones, reacted in 110 DEG C, vacuum under -0.08MPa 8 hours, then 60 DEG C of dischargings are cooled to, esters polymeric monomer is obtained.Then polymerization formula：In four-hole boiling flask, add soft water, then stirring and heating water bath is to 81 83 DEG C of temperature, under this temperature, be added dropwise within 180 minutes mix monomer (wherein mix monomer be esters polymeric monomer/ethers polymeric monomer=0 10,/10 0 monomer), the mixed liquor that constitutes of TGA, soft water, 2.87% ammonium persulfate aqueous solution is added dropwise simultaneously, drip off within 210 minutes, be incubated 1 hour after dripping off, be then cooled to 50 DEG C, 30% sodium hydroxide solution is added, the polycarboxylate water-reducer of the present invention is produced.The present invention can make fresh concrete keep good workability.
Description
Technical field
The present invention relates to the polycarboxylate water-reducer Material Field of concrete.More particularly, the present invention relates to a kind of ester
The preparation method of ether composite polymeric polycarboxylate water-reducer.
Background technology
Polycarboxylate water-reducer is widely used as concrete admixture in concrete.It can improve concrete
Mobility, and the Water usage of concrete can be reduced, therefore intensity and durability of concrete etc. can be improved with a kind of
Effect.When using polycarboxylate water-reducer, in addition to the water-reducing property to concrete is considered, it is also contemplated that newly mixing in operation
The workability of concrete.Mixed mud workability refer to mixed mud mixture be easy to construct and can obtain uniform quality, be molded it is closely knit
Performance.Workability is a comprehensive technical indicator, mainly including mobility, glutinous poly- three aspects of property and water-retaining property, this
Connected each other between three, but be commonly present contradiction.Concrete flowability refers to that concrete stirring thing shakes in dead weight or machinery
Lower produce of the effect of smashing is flowed, the performance of the uniform closely knit full template of stream of energy, and it reflects dilute thick degree of concrete stirring thing and filled
The ability of full template.The overall uniform power that poly- property is concrete mix mixture coarse-fine aggregate in work progress is sticked, is sticked
The good concrete of poly- property can occur without the bad phenomenons such as layering, isolation with mixture in work progress, it is ensured that in concrete
Portion's structure it is uniform.Water-retaining property is that concrete can keep the ability of service behaviour when long-time is static, facilitates scene to apply
Work.So the good polycarboxylate water-reducer of workability is greatly improved for the performance of concrete.
With the development of country, engineering type is increasingly complicated, and the service behaviour for concrete requires also more and more higher.Separately
On the one hand, the particularity and seasonal variations due to lot of domestic and international engineering in application real process are obvious, and material is not
It is same that very big influence can be brought to concrete workability.Therefore, developing a kind of polycarboxylate water-reducer of high workability turns into shape
Gesture is become.
Found by studying, esters polymeric monomer polymerize obtained polycarboxylate water-reducer jointly with ethers polymeric monomer, than pure ester
The polycarboxylate water-reducer that class polymeric monomer or the polymerization of pure ethers polymeric monomer are obtained, in fresh concrete, there is good workability.
The content of the invention
The purpose of the present invention is intended to prepare a kind of polycarboxylate water-reducer of ester ether composite polymeric, can keep fresh concrete
Good workability.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, comprises the following steps：
(1) esters polymeric monomer is prepared：Raw material is according to percentage by weight, and poly glycol monomethyl ether 1000 is 54%, poly- second two
Alcohol monomethyl ether 2000 is that 23%, methacrylic acid accounts for 18%, p-methyl benzenesulfonic acid and accounts for 2%, hydroquinones and accounts for 3%, by above-mentioned raw materials
Reaction vessel is put into, 110 DEG C of esterification temperature of control, vacuum -0.08MPa, 8 hours reaction time, 60 DEG C is then cooled to and goes out
Material, produces the polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of mixing；
(2) mixing polymeric monomer is prepared：The esters polymeric monomer and ethers polymeric monomer for taking step 1 be according to part by weight：Esters
Polymeric monomer/ethers polymeric monomer=0-10/10-0 formation mixing polymeric monomers；Optimal selection is：Esters polymeric monomer：Ethers polymeric monomer=
1：1；
(3) polymerisation：Raw material weighs soft water 34.5% according to percentage by weight, mixes polymeric monomer 38%, TGA
0.33%, 2.87% ammonium persulfate aqueous solution 20%, 30% sodium hydroxide solution 7.17% is stirred equipped with thermometer, speed governing
Mix device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, be firstly added soft water, then stirring and heating water bath are to temperature
81-83 DEG C, under this temperature, the mixed liquor that esters polymeric monomer, TGA, soft water are constituted was dripped with 180 minutes, simultaneously
2.87% ammonium persulfate aqueous solution is added dropwise, drips off within 210 minutes, then insulation 1 hour after dripping off is cooled to 50 DEG C, addition
30% sodium hydroxide solution, produces the polycarboxylate water-reducer of the present invention.
Wherein, ethers polymeric monomer is isoprene alcohol APEO 2400.
Beneficial effects of the present invention：The present invention can make fresh concrete keep good workability.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment one
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, comprises the following steps：
The preparation of esters polymeric monomer：In equipped with thermometer, oil bath pan, speed-adjustable stir device, the three-necked flask of vacuum plant
Add 108 grams of poly glycol monomethyl ethers 1000,46 grams of poly glycol monomethyl ethers 2000,36 grams of methacrylic acids, 4 grams to toluene sulphur
Acid, 5 grams of hydroquinones react 8 hours in 110 DEG C, vacuum under -0.06MPa, are then cooled to 60 DEG C of dischargings, produce mixed
The polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of conjunction.
Polymerization formula：Equipped with thermometer, speed-adjustable stir device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, plus
Enter 75 grams of soft water, then stirring and heating water bath is to 81-83 DEG C of temperature, under this temperature, mixed liquor was dripped with 180 minutes
(mixed liquor that 114 grams, 0.98 gram TGA of esters polymeric monomer of above-mentioned preparation, 28.5 grams of soft water are constituted), is added dropwise simultaneously
2.87% 60 grams of ammonium persulfate aqueous solution, is dripped off for 210 minutes, insulation 1 hour after dripping off, and is then cooled to 50 DEG C, addition
30% 21.52 grams of sodium hydroxide solution, produces the polycarboxylate water-reducer of the present invention.
Embodiment two
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, comprises the following steps：
The preparation of esters polymeric monomer：In equipped with thermometer, oil bath pan, speed-adjustable stir device, the three-necked flask of vacuum plant
Add 108 grams of poly glycol monomethyl ethers 1000,46 grams of poly glycol monomethyl ethers 2000,36 grams of methacrylic acids, 4 grams to toluene sulphur
Acid, 6 grams of hydroquinones react 8 hours in 110 DEG C, vacuum under -0.06MPa, are then cooled to 60 DEG C of dischargings, produce mixed
The polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of conjunction.
Polymerization formula：Equipped with thermometer, speed-adjustable stir device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, plus
Enter 75 grams of soft water, 34.2 grams of isoprene alcohol APEOs 2400, then stirring and heating water bath be to 81-83 DEG C of temperature,
Under this temperature, with drip within 180 minutes mixed liquor (79.8 grams, 0.98 gram TGA of esters polymeric monomer of above-mentioned preparation,
The mixed liquor of 28.5 grams of soft water compositions), while 60 grams of 2.87% ammonium persulfate aqueous solution is added dropwise, drip off within 210 minutes, after dripping off
Insulation 1 hour, is then cooled to 50 DEG C, adds 21.52 grams of 30% sodium hydroxide solution, produces the polycarboxylic acids diminishing of the present invention
Agent.
Embodiment three
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, comprises the following steps：
The preparation of esters polymeric monomer：In equipped with thermometer, oil bath pan, speed-adjustable stir device, the three-necked flask of vacuum plant
Add 108 grams of poly glycol monomethyl ethers 1000,46 grams of poly glycol monomethyl ethers 2000,36 grams of methacrylic acids, 4 grams to toluene sulphur
Acid, 6 grams of hydroquinones react 8 hours in 110 DEG C, vacuum under -0.06MPa, are then cooled to 60 DEG C of dischargings, produce mixed
The polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of conjunction.
Polymerization formula：Equipped with thermometer, speed-adjustable stir device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, plus
Enter 75 grams of soft water, 57 grams of isoprene alcohol APEOs 2400, then stirring and heating water bath are to 81-83 DEG C of temperature, herein
Under temperature, with drip within 180 minutes mixed liquor (57 grams, 0.98 gram TGA of esters polymeric monomer of above-mentioned preparation, 28.5 grams
The mixed liquor of soft water composition), while 60 grams of 2.87% ammonium persulfate aqueous solution is added dropwise, drip off within 210 minutes, insulation 1 after dripping off
Hour, 50 DEG C are then cooled to, 21.52 grams of 30% sodium hydroxide solution is added, the polycarboxylate water-reducer of the present invention is produced.
Example IV
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, comprises the following steps：
The preparation of esters polymeric monomer：In equipped with thermometer, oil bath pan, speed-adjustable stir device, the three-necked flask of vacuum plant
Add 108 grams of poly glycol monomethyl ethers 1000,46 grams of poly glycol monomethyl ethers 2000,36 grams of methacrylic acids, 4 grams to toluene sulphur
Acid, 6 grams of hydroquinones react 8 hours in 110 DEG C, vacuum under -0.06MPa, are then cooled to 60 DEG C of dischargings, produce mixed
The polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of conjunction.
Polymerization formula：Equipped with thermometer, speed-adjustable stir device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, plus
Enter 75 grams of soft water, 79.8 grams of isoprene alcohol APEOs 2400, then stirring and heating water bath be to 81-83 DEG C of temperature,
Under this temperature, with drip within 180 minutes mixed liquor (34.2 grams, 0.98 gram TGA of esters polymeric monomer of above-mentioned preparation,
The mixed liquor of 28.5 grams of soft water compositions), while 60 grams of 2.87% ammonium persulfate aqueous solution is added dropwise, drip off within 210 minutes, after dripping off
Insulation 1 hour, is then cooled to 50 DEG C, adds 21.52 grams of 30% sodium hydroxide solution, produces the polycarboxylic acids diminishing of the present invention
Agent.
Embodiment five
A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, comprises the following steps：
The preparation of esters polymeric monomer：In equipped with thermometer, oil bath pan, speed-adjustable stir device, the three-necked flask of vacuum plant
Add 108 grams of poly glycol monomethyl ethers 1000,46 grams of poly glycol monomethyl ethers 2000,36 grams of methacrylic acids, 4 grams to toluene sulphur
Acid, 6 grams of hydroquinones react 8 hours in 110 DEG C, vacuum under -0.06MPa, are then cooled to 60 DEG C of dischargings, produce mixed
The polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of conjunction.
Polymerization formula：Equipped with thermometer, speed-adjustable stir device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, plus
Enter 75 grams of soft water, 114 grams of isoprene alcohol APEOs 2400, then stirring and heating water bath are to 81-83 DEG C of temperature, herein
Under temperature, mixed liquor (mixed liquor that 0.98 gram of TGA, 28.5 grams of soft water are constituted) was dripped with 180 minutes, is dripped simultaneously
Plus 60 grams of 2.87% ammonium persulfate aqueous solution, drip off within 210 minutes, then insulation 1 hour after dripping off is cooled to 50 DEG C, addition
30% 21.52 grams of sodium hydroxide solution, produces the polycarboxylate water-reducer of the present invention.
Embodiment is evaluated and state description：
Concrete formulation ratio：Golden peak cement p.o42.5：350；Sand：850；Gravelstone：350；Great Shi：700, water reducer 14；
Water：1450.
By above-mentioned evaluation, the polycarboxylate water-reducer that esters polymeric monomer is obtained when polymerizeing with ethers polymeric monomer by 1/1, new
In mixed concrete, there is good workability.
Above content is only citing made for the present invention and explanation, and affiliated those skilled in the art are to being retouched
The specific embodiment stated is made various modifications or supplement or substituted using similar mode, without departing from the design of invention
Or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (2)
1. a kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer, it is characterised in that comprise the following steps：
(1) esters polymeric monomer is prepared：Raw material is according to percentage by weight, and poly glycol monomethyl ether 1000 is 54%, polyethyleneglycol
Methyl ether 2000 is that 23%, methacrylic acid accounts for 18%, p-methyl benzenesulfonic acid and accounts for 2%, hydroquinones and accounts for 3%, and above-mentioned raw materials are put into
Reaction vessel, 110 DEG C of esterification temperature of control, vacuum -0.08MPa, 8 hours reaction time, is then cooled to 60 DEG C of dischargings,
Produce the polyethylene glycol monomethyl ethermethacrylic acid esters polymeric monomer of mixing；
(2) mixing polymeric monomer is prepared：The esters polymeric monomer and ethers polymeric monomer for taking step 1 be according to part by weight：The big list of esters
Body/ethers polymeric monomer=0-10/10-0 formation mixing polymeric monomers；
(3) polymerisation：Raw material weighs soft water 34.5% according to percentage by weight, mixes polymeric monomer 38%, TGA
0.33%, 2.87% ammonium persulfate aqueous solution 20%, 30% sodium hydroxide solution 7.17% is stirred equipped with thermometer, speed governing
Mix device, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, be firstly added soft water, then stirring and heating water bath are to temperature
81-83 DEG C, under this temperature, the mixed liquor that esters polymeric monomer, TGA, soft water are constituted was dripped with 180 minutes, simultaneously
2.87% ammonium persulfate aqueous solution is added dropwise, drips off within 210 minutes, then insulation 1 hour after dripping off is cooled to 50 DEG C, addition
30% sodium hydroxide solution, produces the polycarboxylate water-reducer of the present invention.
2. a kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer as claimed in claim 1, it is characterised in that the ether
Class polymeric monomer is isoprene alcohol APEO 2400.
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| CN201710339643.2A CN107189026A (en) | 2017-05-15 | 2017-05-15 | A kind of preparation method of ester ether composite polymeric polycarboxylate water-reducer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279553A (en) * | 2020-09-28 | 2021-01-29 | 浙江玖龙新材料有限公司 | Ester polycarboxylate superplasticizer formula and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000169206A (en) * | 1998-11-30 | 2000-06-20 | Taiheiyo Cement Corp | Powdery cement dispersant and its production and cement mixture |
| CN102660037A (en) * | 2012-04-11 | 2012-09-12 | 长沙加美乐素化工有限公司 | Preparation method of super-sustained release ester-ether crosslinking polycarboxylic acid water reducer |
| CN102746438A (en) * | 2011-04-27 | 2012-10-24 | 江苏尼高科技有限公司 | Preparation method of polycarboxylic acids water reducer |
-
2017
- 2017-05-15 CN CN201710339643.2A patent/CN107189026A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000169206A (en) * | 1998-11-30 | 2000-06-20 | Taiheiyo Cement Corp | Powdery cement dispersant and its production and cement mixture |
| CN102746438A (en) * | 2011-04-27 | 2012-10-24 | 江苏尼高科技有限公司 | Preparation method of polycarboxylic acids water reducer |
| CN102660037A (en) * | 2012-04-11 | 2012-09-12 | 长沙加美乐素化工有限公司 | Preparation method of super-sustained release ester-ether crosslinking polycarboxylic acid water reducer |
Non-Patent Citations (2)
| Title |
|---|
| 王子明: "《"聚羧酸系高性能减水剂-制备•性能与应用"》", 30 June 2009, 中国建筑工业出版社 * |
| 黄靖等: "《聚羧酸系高性能减水剂及其应用技术新进展—2015》", 31 May 2015, 北京理工大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279553A (en) * | 2020-09-28 | 2021-01-29 | 浙江玖龙新材料有限公司 | Ester polycarboxylate superplasticizer formula and preparation method |
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