CN109705283B - Retarding polycarboxylate superplasticizer and preparation method thereof - Google Patents
Retarding polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 32
- 230000000979 retarding effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000008030 superplasticizer Substances 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 30
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 12
- 229920000570 polyether Polymers 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 8
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical group OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 4
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims 1
- 239000004568 cement Substances 0.000 abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000013329 compounding Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010276 construction Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- -1 pebble Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the field of water reducing agents, and particularly discloses a retarding polycarboxylate water reducing agent and a preparation method thereof. The retarding polycarboxylate superplasticizer is prepared from the following components in percentage by weight: 20 to 45 percent of unsaturated polyether, 2 to 6 percent of unsaturated acid, 0.9 to 10 percent of sodium p-styrene sulfonate, 0.5 to 2 percent of organic phosphoric acid, 0.2 to 1 percent of oxidant, 0.05 to 0.2 percent of reducing agent, 0.1 to 0.5 percent of chain transfer agent and the balance of water. The retarding polycarboxylate superplasticizer has high water reducing rate and good retarding effect, has good adaptability to different varieties of cement, and does not produce side effect due to different varieties of cement. In addition, the slow-setting polycarboxylate superplasticizer has a good anticorrosion effect, and the polycarboxylate superplasticizer cannot rot, delaminate, smell and the like due to overlong standing time in summer.
Description
Technical Field
The invention belongs to the field of water reducing agents, and particularly discloses a retarding polycarboxylate water reducing agent and a preparation method thereof.
Background
The retarding water reducer is an admixture with wide application range in concrete admixture, and has retarding and greatly reduced water consumption. As the basic construction development puts more and higher requirements on the performance of concrete, higher requirements on concrete admixtures are also put forward.
The high-performance polycarboxylate superplasticizer has the advantages of high water reducing rate, good cement dispersibility and small concrete slump loss. However, the polycarboxylate superplasticizers themselves have a relatively weak retarding effect, and the above-mentioned effect must be achieved by compounding with a retarder. Although the compounding technology can solve part of problems, the degree of solving the problems by compounding is limited, the original water reducing performance of the water reducing agent is sacrificed, and the cost is increased by additionally adding the retarder. In addition, the water reducing agent solution of the compound retarder can also have the phenomena of layering, precipitation, putrefaction, odor generation and the like, and the stability of the product performance is worried. Therefore, the development of a high-performance water reducing agent which has high water reducing rate, obvious retardation effect, stable product performance and ideal later reinforcing effect on concrete is urgently needed.
Disclosure of Invention
The invention aims to overcome the defects that the existing polycarboxylate superplasticizer cannot take water reducing and retarding into consideration and the performance of the polycarboxylate superplasticizer is influenced by compounding the existing polycarboxylate superplasticizer with the existing retarder, and provides the polycarboxylate superplasticizer which can take water reducing and retarding into consideration and a preparation method thereof.
The invention particularly provides a retarding polycarboxylate superplasticizer which is prepared from the following components in percentage by weight:
preferably, the retarding polycarboxylate superplasticizer is prepared from the following components in percentage by weight:
preferably, the unsaturated polyether is an isobutylene-based polyoxyethylene ether.
Preferably, the unsaturated polyether has a number average molecular weight of 600-3000, more preferably 2400-3000.
Preferably, the unsaturated acid is acrylic acid and/or methacrylic acid.
Preferably, the organophosphonic acid is hydroxyethylidene diphosphonic acid and/or aminotrimethylidene phosphonic acid.
Preferably, the oxidizing agent is potassium persulfate and/or ammonium persulfate.
Preferably, the reducing agent is ascorbic acid and/or tartaric acid.
Preferably, the chain transfer agent is thioglycolic acid and/or mercaptopropionic acid.
The invention also provides a preparation method of the retarding polycarboxylate superplasticizer, which comprises the following steps:
(1) preparing 45-55 wt% aqueous solution of sodium p-styrene sulfonate and unsaturated acid, and marking as a first solution, and preparing 3-10 wt% aqueous solution of reducing agent and chain transfer agent, and marking as a second solution;
(2) preparing the unsaturated polyether into an aqueous solution with the concentration of 35-45 wt%, adding the oxidant, then simultaneously dropwise adding the first solution and the second solution, adding the organic phosphoric acid after dropwise adding is finished, continuing to react for 0.5-2 h, and supplementing a certain amount of water after the reaction is finished to obtain a slow-setting polycarboxylic acid water reducer solution with the concentration of 40 wt%.
Preferably, the total time for dripping the first solution and the second solution is controlled within 2-3 h.
In addition, the invention also provides the retarding polycarboxylate superplasticizer prepared by the method.
The key point of the invention is that the unsaturated polyether, the unsaturated acid, the sodium p-styrene sulfonate and the organic phosphoric acid are used in a matching way according to specific dosage, especially the dosage of the sodium p-styrene sulfonate is increased, and the invention has the following beneficial effects:
(1) the retarding polycarboxylate superplasticizer has high water reducing rate and good retarding effect, has better adaptability with different varieties of cement, and does not generate side effect due to different varieties of cement;
(2) the slow-setting polycarboxylate superplasticizer has a good corrosion prevention effect, and can not be rotten, layered, smelly and the like due to overlong standing time in summer.
(3) The preparation process of the retarding polycarboxylate superplasticizer is simple, the reaction is carried out at normal temperature, the temperature in the whole process is not required to be controlled, the reaction time is short, the energy consumption is low, the safety coefficient is high, no pollution is caused, and the industrial production is easy to realize.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative of the invention and is not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
Raw materials: see table 1.
The preparation process comprises the following steps:
(1) preparing 50 wt% aqueous solution of sodium p-styrene sulfonate and unsaturated acid, and marking as a first solution, and preparing 5.5 wt% aqueous solution of reducing agent and chain transfer agent, and marking as a second solution;
(2) preparing unsaturated polyether into a 40wt% aqueous solution, adding an oxidant, then simultaneously dropwise adding the first solution and the second solution, controlling the total dropwise adding time to be 2-3 h, adding organic phosphoric acid after the dropwise adding is finished, and continuing to react for 1 h. After the reaction is finished, a certain amount of water is supplemented to obtain a retarding polycarboxylate superplasticizer solution with the concentration of 40 wt%.
Example 2
Raw materials: see table 1.
The preparation method is the same as that of example 1.
Example 3
Raw materials: see table 1.
The preparation method is the same as that of example 1.
Example 4
Raw materials: see table 1.
The preparation method is the same as that of example 1.
Example 5
Raw materials: see table 1.
The preparation method is the same as that of example 1.
Comparative example 1
Raw materials: the difference from example 2 is that the amount of sodium p-styrene sulfonate is reduced to 0.5 wt%, as shown in Table 1.
The preparation method is the same as that of example 1.
Comparative example 2
Raw materials: the difference from example 2 is that no organic phosphoric acid is added, as shown in Table 1.
The preparation method is the same as that of example 1.
TABLE 1 ingredient tables (unit: parts by weight) used in examples
Effect verification
(1) The net slurry fluidity of each of the examples and comparative examples at the same blending amount was measured by using the whelk p.o42.5 cement, the jianfu p.o42.5 cement and the minfu p.ii 42.5 cement. The test is carried out according to GB/T8077-2012 'concrete admixture homogeneity test method', the W/C is 2.9, the cement is 300g, the water is 87g, and the admixture mixing amount is the folded solid mixing amount. The test results are shown in Table 2.
TABLE 2 Net paste fluidity Performance results for different water reducer types
As can be seen from Table 2, the 1h cement paste fluidity loss of the retarding polycarboxylate water reducer in the example is smaller than that of the comparative example in different cements.
(2) Concrete test
The initial and final setting times of the concrete are tested by adopting Fujian cement and conch cement, and the test is carried out according to GB/T50080-2002 Standard of Performance test methods of concrete mixtures. The design label of the concrete is C30, the mix proportion of the concrete is that cement, water, sand, pebble, fly ash and mineral powder are 258, 170, 815, 996, 41 and 41 by weight, and the mixing amount of the water reducing agent is the mixing amount of the bending and fixing agent, calculated by the mass of the cement, the fly ash and the mineral powder. The test results are shown in Table 3.
TABLE 3 concrete setting time and compression strength meter (test temperature 20 deg.C)
The data in the table show that the retarding water reducer provided by the invention not only has higher water reducing rate, but also can prolong the setting time of concrete, and the compressive strength of the concrete in 7 days and 28 days can meet the construction requirements.
(4) The anticorrosion effect is as follows:
three samples of example 4, comparative example 1 and comparative example 2 were placed in numbers 1, respectively#、2#、3#Three stoppered tubes of (1) and stored in the laboratory (room temperature 30 ℃), and found 3 after one month#With slight floc, 1#、2#There was no change. Observed two months later, 3#With an odor and a pronounced floc precipitate, 1#And 2#The samples in these two tubes were unchanged. Therefore, the addition of the organic phosphoric acid can slow or prevent the deterioration and deterioration of the water reducing agent.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (8)
1. A preparation method of a retarding polycarboxylate superplasticizer is characterized by comprising the following steps:
(1) preparing 45-55 wt% aqueous solution of sodium p-styrene sulfonate and unsaturated acid, and marking as a first solution, and preparing 3-10 wt% aqueous solution of a reducing agent and a chain transfer agent, and marking as a second solution;
(2) preparing unsaturated polyether into an aqueous solution with the concentration of 35-45 wt%, adding an oxidant, then simultaneously dropwise adding the first solution and the second solution, adding organic phosphonic acid after dropwise adding is finished, continuing to react for 0.5-2 h, and supplementing a certain amount of water after the reaction is finished to obtain a retarding polycarboxylate water reducer solution with the concentration of 40 wt%;
the weight percentage of each raw material is as follows:
20 to 45 percent of unsaturated polyether;
2 to 6 percent of unsaturated acid;
4.1 to 10 percent of sodium p-styrene sulfonate;
0.5 to 2 percent of organic phosphonic acid;
0.2 to 1 percent of oxidant;
0.05 to 0.2 percent of reducing agent;
0.1 to 0.5 percent of chain transfer agent;
the balance of water;
the unsaturated polyether is isobutylene polyoxyethylene ether; the organic phosphonic acid is hydroxyethylidene diphosphonic acid and/or amino trimethylene phosphonic acid.
2. The preparation method of the slow-setting polycarboxylate water reducer according to claim 1, characterized in that the total time for dripping the first solution and the second solution is controlled within 2-3 h.
3. The preparation method of the retarding polycarboxylate water reducer according to claim 1, characterized in that the weight percentages of the raw materials are as follows:
25 to 35 percent of unsaturated polyether;
2.5 to 4 percent of unsaturated acid;
4.1 to 7 percent of sodium p-styrene sulfonate;
0.7 to 1.5 percent of organic phosphonic acid;
0.25 to 0.65 percent of oxidant;
0.06 percent to 0.15 percent of reducing agent;
0.1 to 0.4 percent of chain transfer agent;
the balance being water.
4. The method for preparing the retarding polycarboxylate water reducer according to any one of claims 1-3, wherein the number average molecular weight of the unsaturated polyether is 600-3000.
5. The preparation method of the slow-setting polycarboxylate water reducer as claimed in claim 4, wherein the number average molecular weight of the unsaturated polyether is 2400-3000.
6. The preparation method of the retarding polycarboxylate water reducer according to any one of claims 1-3, characterized in that the unsaturated acid is acrylic acid and/or methacrylic acid.
7. The preparation method of the retarding polycarboxylate water reducer according to any one of claims 1-3, characterized in that the oxidant is potassium persulfate and/or ammonium persulfate; the reducing agent is ascorbic acid and/or tartaric acid; the chain transfer agent is thioglycolic acid and/or mercaptopropionic acid.
8. The retarding polycarboxylate water reducer prepared by the method of any one of claims 1-7.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1289736A (en) * | 1999-11-17 | 2001-04-04 | 武汉水利电力大学 | High-efficiency water-reducing, retarding and plastic-retaining agent for concrete |
| CN103848944A (en) * | 2013-05-14 | 2014-06-11 | 科之杰新材料集团有限公司 | Preparation method of super-retarding type polycarboxylate superplasticizer |
| CN105254825A (en) * | 2015-11-18 | 2016-01-20 | 科之杰新材料集团有限公司 | Preparation method of esters retarding polycarboxylic acid slump retaining agent |
| CN106116232A (en) * | 2016-06-24 | 2016-11-16 | 桂林华越环保科技有限公司 | A kind of anti-freezing concrete water reducer |
| CN107987227A (en) * | 2017-12-07 | 2018-05-04 | 科之杰新材料集团有限公司 | A kind of preparation method of low hydration heat extra retarded set type polycarboxylate water-reducer |
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| US5890840A (en) * | 1995-12-08 | 1999-04-06 | Carter, Jr.; Ernest E. | In situ construction of containment vault under a radioactive or hazardous waste site |
| CN103183792B (en) * | 2011-12-27 | 2015-04-29 | 山西黄腾化工有限公司 | Preparation method of polycarboxylic water reducer |
| JP6832773B2 (en) * | 2016-03-31 | 2021-02-24 | 株式会社日本触媒 | Admixture material composition |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1289736A (en) * | 1999-11-17 | 2001-04-04 | 武汉水利电力大学 | High-efficiency water-reducing, retarding and plastic-retaining agent for concrete |
| CN103848944A (en) * | 2013-05-14 | 2014-06-11 | 科之杰新材料集团有限公司 | Preparation method of super-retarding type polycarboxylate superplasticizer |
| CN105254825A (en) * | 2015-11-18 | 2016-01-20 | 科之杰新材料集团有限公司 | Preparation method of esters retarding polycarboxylic acid slump retaining agent |
| CN106116232A (en) * | 2016-06-24 | 2016-11-16 | 桂林华越环保科技有限公司 | A kind of anti-freezing concrete water reducer |
| CN107987227A (en) * | 2017-12-07 | 2018-05-04 | 科之杰新材料集团有限公司 | A kind of preparation method of low hydration heat extra retarded set type polycarboxylate water-reducer |
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