CN104311752A - Polycarboxylic acid water reducer and preparation method thereof - Google Patents
Polycarboxylic acid water reducer and preparation method thereof Download PDFInfo
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- CN104311752A CN104311752A CN201410531624.6A CN201410531624A CN104311752A CN 104311752 A CN104311752 A CN 104311752A CN 201410531624 A CN201410531624 A CN 201410531624A CN 104311752 A CN104311752 A CN 104311752A
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Abstract
The invention discloses a polycarboxylic acid water reducer and a preparation method thereof. Raw materials of the polycarboxylic acid water reducer comprise the following components in parts by weight: 160-170 parts of an ether-based monomer having a molecular weight of 600-3000, 1-4 parts of an unsaturated phosphorous-containing monomer, 1-3 parts of an unsaturated silicon-containing monomer, 15-25 parts of acrylic acid, 1-2 parts of an oxidant, 2-2.5 parts of sodium hypophosphite, 0.3-1.0 part of promoter and 250 parts of water. Since unsaturated phosphorous-containing and silicon-containing monomers are added into the raw materials of the polycarboxylic acid water reducer, a plurality of phosphorous-containing and silicon-containing groups are introduced into molecular chains of the water reducer, so that the polycarboxylic acid water reducer having the advantages of high water-reducing rate, good slump-retaining property and facilitation in development of early strength of concrete is prepared and the common problems of low water-reducing rate and poor slump-retaining property when the polycarboxylic acid water reducer is applied in machine-made sand are overcome.
Description
Technical field
The invention belongs to building material technical field, be specifically related to a kind of polycarboxylate water-reducer and preparation method thereof.
Background technology
Polycarboxylate water-reducer is as novel water reducer, have that volume is low, water-reducing rate is high, slump-retaining good, shrinking percentage is little, relative with adulterant adaptability with cement better, a series of outstanding performance such as reinforced effects is obvious, be widely used at present in every engineering field.
Sand is concrete important composition material, although national standard and industry standard are all to its silt content, clod content's index has strict restriction, because the Area distribution of natural resources is different, there is a great difference in various places Sand for Concrete, comprise: river sand, the mixed sand of Machine-made Sand and river sand and Machine-made Sand composition, wherein the silt content of Machine-made Sand is higher, Machine-made Sand application in recent years increases, but poly carboxylic acid series water reducer is comparatively responsive to the silt content of aggregate, main manifestations is increasing along with sand silt content, the diminishing dispersive ability degradation of poly carboxylic acid series water reducer, guarantor is collapsed weak effect, cause the problems such as maturing intensity reduction.Therefore, polycarboxylate water-reducer is applied in Machine-made Sand, and the low problem with protecting collapsing property difference of ubiquity water-reducing rate, can not ensure concrete construction quality.
In addition in recent years, the various synthesis techniques of polycarboxylate water-reducer emerge in an endless stream, the monomers such as methacrylic Soxylat A 25-7 and vinylformic acid, maleic anhydride dimethyl ester, methylpropene sodium sulfonate gather by CN 103553409A under the effect of molecular weight chain oxygenant, chain-transfer agent Thiovanic acid or thiohydracrylic acid, obtain a kind of polycarboxylate water-reducer.CN 103723945 A is by double bond containing polyether monomer, double bond containing carboxylic acid monomer and water-soluble micro-crosslinked functional agent, in the presence of water-soluble oxidizers and chain-transfer agent, after aqueous solution polymerization reaction, and regulate reaction system pH to be 7 ~ 8 with alkali, be hydrolyzed sustained-release polycarboxylic water reducer soon, its Chain transfer agent is mercaptoethanol, 2-hydroxyl propylmercaptan, Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid, one or several mixtures in any proportion of 2-dimercaptosuccinic acid.The chain-transfer agent used in visible most of technique is the sulfydryl such as Thiovanic acid, thiohydracrylic acid class starting material, and such starting material taste weight is unfavorable to the operation of environment and industrial workman.
Summary of the invention
The object of the invention is to overcome prior art defect, a kind of polycarboxylate water-reducer is provided.
Another object of the present invention is to the preparation method that above-mentioned polycarboxylate water-reducer is provided.
Concrete technical scheme of the present invention is as follows:
A kind of polycarboxylate water-reducer, its raw material comprises the component of following weight part:
Described ether type monomer is at least one in methacrylic polyoxyethylene poly-oxygen propylene aether (HPEG) and isopentene group polyoxyethylene poly-oxygen propylene aether (TPEG);
Described unsaturated be at least one in isopropylene and phosphonic acid, 2 ~ acrylamide ~ 2 ~ methyl-propyl phosphonic acids and ethylene diamine ~ dimethyl phosphonic acids containing phosphine monomer;
Described unsaturated silicon-containing monomer is at least one in vinyltrimethoxy silane, vinyltriethoxysilane and vinyl silane triisopropoxide
In a preferred embodiment of the invention, its raw material comprises the component of following weight part:
In a preferred embodiment of the invention, described oxygenant is hydrogen peroxide, Potassium Persulphate, Sodium Persulfate or ammonium persulphate.
In a preferred embodiment of the invention, described promotor is at least one in iron protochloride and ferrous sulfate.
A preparation method for above-mentioned polycarboxylate water-reducer, comprises the steps:
(1) by ether type monomer, unsaturatedly to join together with water in reactor containing phosphine monomer, unsaturated silicon-containing monomer, at 5-40 DEG C after stirring and dissolving, drip aqueous oxidizing agent solution and vinylformic acid, sodium hypophosphite and promotor mixed aqueous solution respectively, time for adding is 2 ~ 4 hours, drips and terminates rear constant temperature 1 ~ 2 hour;
(2) copolyreaction: after copolyreaction terminates, by alkaline matter adjusted to ph in the scope of 6.0-7.0, obtains settled solution and is described polycarboxylate water-reducer.
In a preferred embodiment of the invention, described step (1) is:: by ether type monomer, unsaturatedly to join together with water in reactor containing phosphine monomer, unsaturated silicon-containing monomer, at 5-35 DEG C after stirring and dissolving, drip aqueous oxidizing agent solution and vinylformic acid, sodium hypophosphite and promotor mixed aqueous solution respectively, time for adding is 2.5 ~ 4 hours, drips and terminates rear constant temperature 1 ~ 1.5 hour.
In a preferred embodiment of the invention, described alkaline matter is at least one in sodium hydroxide, calcium hydroxide, potassium hydroxide, calcium oxide, ammoniacal liquor and trolamine.
The invention has the beneficial effects as follows:
Some are added unsaturated containing phosphine, silicon-containing monomer in the raw material of 1, polycarboxylate water-reducer of the present invention, thus in water reducer molecular chain, introduce some containing phosphine, silicon-containing group, prepare that a kind of water-reducing rate is high, slump retaining good, be beneficial to the polycarboxylate water-reducer of early age strength of concrete development, overcoming polycarboxylate water-reducer is applied in Machine-made Sand, the low problem with protecting collapsing property difference of ubiquity water-reducing rate.
Sodium hypophosphite in the raw material of 2, polycarboxylate water-reducer of the present invention can form redox initiation system with oxygenant, can play again the effect of chain-transfer agent, avoid the use of traditional chain transfer agent, be beneficial to and improve production plant environment, environmental protection.
Embodiment
Be further detailed below by way of embodiment technical scheme of the present invention and describe.
Embodiment 1
(1) each feed composition is taken by following proportioning:
(2) copolyreaction: TPEG, isopropylene and phosphonic acid, vinyltrimethoxy silane are joined in reactor together with 190 weight parts waters, at 5 ~ 35 DEG C after stirring and dissolving, drip the mixed aqueous solution (vinylformic acid, iron protochloride, sodium hypophosphite and 30 weight parts waters) of sodium persulfate aqueous solution (Sodium Persulfate and 30 weight parts waters) and vinylformic acid, sodium hypophosphite and iron protochloride respectively, time for adding is 2.5 hours, dropping terminates rear constant temperature 1.5 hours, and reaction products therefrom concentration is about 40%;
(3) after copolyreaction terminates, by sodium hydroxide adjusted to ph in the scope of 6.0 ~ 7.0, obtain settled solution and be described polycarboxylate water-reducer.
Embodiment 2
(1) each feed composition is taken by following proportioning:
(2) copolyreaction: TPEG, 2-acrylamide-2-methyl-propyl phosphonic acids, vinyltriethoxysilane are joined in reactor together with 190 weight parts waters, at 5 ~ 35 DEG C after stirring and dissolving, drip the mixed aqueous solution (vinylformic acid, ferrous sulfate, sodium hypophosphite and 30 weight parts waters) of ammonium persulfate aqueous solution (ammonium persulphate and 30 weight parts waters) and vinylformic acid, sodium hypophosphite and iron protochloride respectively, time for adding is 3 hours, dropping terminates rear constant temperature 1 hour, and reaction products therefrom concentration is about 40%;
(3) after copolyreaction terminates, by potassium hydroxide adjusted to ph in the scope of 6.0 ~ 7.0, obtain settled solution and be described polycarboxylate water-reducer.
Embodiment 3
(1) each feed composition is taken by following proportioning:
(2) copolyreaction: HPEG, ethylene diamine-dimethyl phosphonic acids, vinyl silane triisopropoxide are joined in reactor together with 190 weight parts waters, at 5 ~ 35 DEG C after stirring and dissolving, dripped the mixed aqueous solution (vinylformic acid, iron protochloride, ferrous sulfate, sodium hypophosphite and 30 weight parts waters) of aqueous hydrogen peroxide solution (hydrogen peroxide and 30 weight parts waters) and vinylformic acid, sodium hypophosphite, iron protochloride and ferrous sulfate respectively, time for adding is 4 hours, dropping terminates rear constant temperature 1 hour, and reaction products therefrom concentration is about 40%;
(3) after copolyreaction terminates, by trolamine adjusted to ph in the scope of 6.0 ~ 7.0, obtain settled solution and be described polycarboxylate water-reducer.
Embodiment 4
By the polycarboxylate water-reducer of embodiment 1-3 gained and contrast sample (standard type polycarboxylate water-reducer), adopt standard cement, according to GB 8076-2008 " concrete admixture ", when surveying its water-reducing rate and each compressive strength rate in the length of time of concrete, concrete mix is: cement 330kg/m
3, sand 740kg/m
3, stone 1116kg/m
3; When surveying its slump retaining, concrete mix is: cement 360kg/m
3, sand 803kg/m
3, stone 982kg/m
3; Acquired results as shown in Table 1 and Table 2.
Table 1 embodiment water-reducing rate and concrete crushing strength comparison ratio
Table 2 embodiment slump retaining contrasts
Test-results illustrates, environmental type polycarboxylate water-reducer water-reducing rate of the present invention is high, slump retaining good, be beneficial to early age strength of concrete development, can be applicable to need in high diminishing, early strong concrete.Synthesis technique is without the need to heating, and avoid application sulfydryl class chain-transfer agent, be beneficial to and improve production plant environment, production technique is simple, easy control of reaction conditions, energy-saving and cost-reducing, environmental protection.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (7)
1. a polycarboxylate water-reducer, is characterized in that: its raw material comprises the component of following weight part:
Described ether type monomer is at least one in methacrylic polyoxyethylene poly-oxygen propylene aether and isopentene group polyoxyethylene poly-oxygen propylene aether;
Described unsaturated be at least one in isopropylene and phosphonic acid, 2 ~ acrylamide ~ 2 ~ methyl-propyl phosphonic acids and ethylene diamine ~ dimethyl phosphonic acids containing phosphine monomer;
Described unsaturated silicon-containing monomer is at least one in vinyltrimethoxy silane, vinyltriethoxysilane and vinyl silane triisopropoxide.
2. a kind of polycarboxylate water-reducer as claimed in claim 1, is characterized in that: its raw material comprises the component of following weight part:
3. a kind of polycarboxylate water-reducer as claimed in claim 1 or 2, is characterized in that: described oxygenant is hydrogen peroxide, Potassium Persulphate, Sodium Persulfate or ammonium persulphate.
4. a kind of polycarboxylate water-reducer as claimed in claim 1 or 2, is characterized in that: described promotor is at least one in iron protochloride and ferrous sulfate.
5. a preparation method for the polycarboxylate water-reducer in Claims 1-4 described in arbitrary claim, is characterized in that: comprise the steps:
(1) by ether type monomer, unsaturatedly to join together with water in reactor containing phosphine monomer, unsaturated silicon-containing monomer, at 5-40 DEG C after stirring and dissolving, drip aqueous oxidizing agent solution and vinylformic acid, sodium hypophosphite and promotor mixed aqueous solution respectively, time for adding is 2 ~ 4 hours, drips and terminates rear constant temperature 1 ~ 2 hour;
(2) copolyreaction: after copolyreaction terminates, by alkaline matter adjusted to ph in the scope of 6.0-7.0, obtains settled solution and is described polycarboxylate water-reducer.
6. preparation method as claimed in claim 5, it is characterized in that: described step (1) is: by ether type monomer, unsaturatedly to join together with water in reactor containing phosphine monomer, unsaturated silicon-containing monomer, at 5-35 DEG C after stirring and dissolving, drip aqueous oxidizing agent solution and vinylformic acid, sodium hypophosphite and promotor mixed aqueous solution respectively, time for adding is 2.5 ~ 4 hours, drips and terminates rear constant temperature 1 ~ 1.5 hour.
7. the preparation method as described in claim 5 or 6, is characterized in that: described alkaline matter is at least one in sodium hydroxide, calcium hydroxide, potassium hydroxide, calcium oxide, ammoniacal liquor and trolamine.
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Cited By (12)
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| CN105254792A (en) * | 2015-10-19 | 2016-01-20 | 刘剑锋 | Modified cardanol derivative water reducer and preparation method thereof |
| CN107245131A (en) * | 2017-07-10 | 2017-10-13 | 北京工业大学 | The method that amino-polyether end group silanization prepares collapse protective poly-carboxylic acid water reducing agent |
| CN108147700A (en) * | 2017-12-28 | 2018-06-12 | 科之杰新材料集团有限公司 | A kind of preparation method for reducing viscosity reduction type polycarboxylic acids plasticiser |
| CN108218282A (en) * | 2017-12-28 | 2018-06-29 | 科之杰新材料集团有限公司 | A kind of preparation method of anti-mud viscosity reduction type polycarboxylic acids plasticiser |
| CN108349806A (en) * | 2015-11-30 | 2018-07-31 | 罗门哈斯公司 | High solids content polycarboxylate for cement super plasticizer synthesizes |
| CN109232828A (en) * | 2018-09-07 | 2019-01-18 | 科之杰新材料集团有限公司 | A kind of preparation method of ester ether copoly type viscosity reduction type polycarboxylate water-reducer |
| CN109265052A (en) * | 2018-09-07 | 2019-01-25 | 科之杰新材料集团有限公司 | A kind of preparation method being crosslinked viscosity reduction type polycarboxylate water-reducer |
| CN109293847A (en) * | 2018-09-07 | 2019-02-01 | 科之杰新材料集团有限公司 | A kind of preparation method of ethers viscosity reduction type polycarboxylate water-reducer |
| CN109320714A (en) * | 2018-08-29 | 2019-02-12 | 南京博特新材料有限公司 | A kind of dedicated small molecule super plasticizer of middle low-slump concrete and preparation method thereof |
| CN113717313A (en) * | 2021-08-02 | 2021-11-30 | 佳化化学（茂名）有限公司 | Carboxylic acid copolymer and preparation method and application thereof |
| CN113773457A (en) * | 2021-08-26 | 2021-12-10 | 北京工业大学 | Low-creep high-efficiency polycarboxylate superplasticizer and preparation method thereof |
| CN114524637A (en) * | 2021-12-27 | 2022-05-24 | 科之杰新材料集团有限公司 | High-dispersity early-strength polycarboxylate superplasticizer and preparation method thereof |
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| CN105254792A (en) * | 2015-10-19 | 2016-01-20 | 刘剑锋 | Modified cardanol derivative water reducer and preparation method thereof |
| CN108349806A (en) * | 2015-11-30 | 2018-07-31 | 罗门哈斯公司 | High solids content polycarboxylate for cement super plasticizer synthesizes |
| CN108349806B (en) * | 2015-11-30 | 2022-01-25 | 罗门哈斯公司 | Synthesis of high solid content polycarboxylate for cement superplasticizer |
| CN107245131A (en) * | 2017-07-10 | 2017-10-13 | 北京工业大学 | The method that amino-polyether end group silanization prepares collapse protective poly-carboxylic acid water reducing agent |
| CN107245131B (en) * | 2017-07-10 | 2019-03-22 | 北京工业大学 | The method that amino-polyether end group silanization prepares collapse protective poly-carboxylic acid water reducing agent |
| CN108218282B (en) * | 2017-12-28 | 2020-03-06 | 科之杰新材料集团有限公司 | Preparation method of anti-mud viscosity-reducing polycarboxylic acid plasticizer |
| CN108147700A (en) * | 2017-12-28 | 2018-06-12 | 科之杰新材料集团有限公司 | A kind of preparation method for reducing viscosity reduction type polycarboxylic acids plasticiser |
| CN108218282A (en) * | 2017-12-28 | 2018-06-29 | 科之杰新材料集团有限公司 | A kind of preparation method of anti-mud viscosity reduction type polycarboxylic acids plasticiser |
| CN108147700B (en) * | 2017-12-28 | 2020-12-29 | 科之杰新材料集团有限公司 | Preparation method of shrinkage-reducing viscosity-reducing polycarboxylic acid plasticizer |
| CN109320714A (en) * | 2018-08-29 | 2019-02-12 | 南京博特新材料有限公司 | A kind of dedicated small molecule super plasticizer of middle low-slump concrete and preparation method thereof |
| CN109232828A (en) * | 2018-09-07 | 2019-01-18 | 科之杰新材料集团有限公司 | A kind of preparation method of ester ether copoly type viscosity reduction type polycarboxylate water-reducer |
| WO2020048083A1 (en) * | 2018-09-07 | 2020-03-12 | 科之杰新材料集团有限公司 | Preparation method for crosslinked viscosity-reducing polycarboxylic acid water reducer |
| CN109232828B (en) * | 2018-09-07 | 2020-09-04 | 科之杰新材料集团有限公司 | Preparation method of ester ether copolymerization type viscosity reduction type polycarboxylate superplasticizer |
| CN109293847A (en) * | 2018-09-07 | 2019-02-01 | 科之杰新材料集团有限公司 | A kind of preparation method of ethers viscosity reduction type polycarboxylate water-reducer |
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| CN113717313A (en) * | 2021-08-02 | 2021-11-30 | 佳化化学（茂名）有限公司 | Carboxylic acid copolymer and preparation method and application thereof |
| CN113773457A (en) * | 2021-08-26 | 2021-12-10 | 北京工业大学 | Low-creep high-efficiency polycarboxylate superplasticizer and preparation method thereof |
| CN113773457B (en) * | 2021-08-26 | 2022-06-07 | 北京工业大学 | Low-creep high-efficiency polycarboxylate superplasticizer and preparation method thereof |
| CN114524637A (en) * | 2021-12-27 | 2022-05-24 | 科之杰新材料集团有限公司 | High-dispersity early-strength polycarboxylate superplasticizer and preparation method thereof |
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Address after: 361000 Fujian province Xiamen torch hi tech Zone (Xiangan) Industrial Zone neian Road No. 169 Co-patentee after: Kezhijie new material group (Guizhou) Co., Ltd Patentee after: KZJ NEW MATERIALS GROUP Co.,Ltd. Co-patentee after: XIAMEN TIANRUN JINLONG BUILDING MATERIAL Co.,Ltd. Address before: 361000 Fujian province Xiamen torch hi tech Zone (Xiangan) Industrial Zone neian Road No. 169 Co-patentee before: GUIZHOU KZJ NEW MATERIALS Co.,Ltd. Patentee before: KZJ NEW MATERIALS GROUP Co.,Ltd. Co-patentee before: XIAMEN TIANRUN JINLONG BUILDING MATERIAL Co.,Ltd. |