CN115947563A - Polyether air entraining agent and preparation method and application thereof - Google Patents
Polyether air entraining agent and preparation method and application thereof Download PDFInfo
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- CN115947563A CN115947563A CN202211339614.3A CN202211339614A CN115947563A CN 115947563 A CN115947563 A CN 115947563A CN 202211339614 A CN202211339614 A CN 202211339614A CN 115947563 A CN115947563 A CN 115947563A
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- sulfamic acid
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- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 65
- 229920000570 polyether Polymers 0.000 title claims abstract description 65
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000004567 concrete Substances 0.000 claims abstract description 45
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 22
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 238000012216 screening Methods 0.000 claims abstract description 19
- 239000006260 foam Substances 0.000 claims abstract description 17
- 239000003381 stabilizer Substances 0.000 claims abstract description 15
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002474 experimental method Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 238000005187 foaming Methods 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 238000012512 characterization method Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 238000005457 optimization Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 229920002050 silicone resin Polymers 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 239000004574 high-performance concrete Substances 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229930182490 saponin Natural products 0.000 description 2
- 150000007949 saponins Chemical class 0.000 description 2
- 235000017709 saponins Nutrition 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- 238000009435 building construction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 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
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Degasification And Air Bubble Elimination (AREA)
Abstract
The invention belongs to the technical field of concrete admixtures, and discloses a polyether air entraining agent, a preparation method and application thereof, wherein a single-factor experiment is utilized to screen the optimal mixture ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer; screening the optimal preparation parameters, and weighing fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer according to the screened optimal proportion; putting the weighed fatty alcohol-polyoxyethylene ether, sulfamic acid and catalyst into a flask under the condition of nitrogen protection, and stirring continuously; and heating the flask, reacting at constant temperature for a certain time, cooling, adding the modified silicon resin polyether microemulsion, and fully and uniformly stirring to obtain the polyether air entraining agent. The high-performance concrete polyether air entraining agent prepared and synthesized by the invention can improve the workability and the homogeneity of concrete, improve the frost resistance of the concrete and greatly improve the comprehensive durability of the concrete.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a polyether air entraining agent, a preparation method and application thereof.
Background
At present, the admixture has a very important position in concrete materials, the air entraining agent is widely applied to concrete as an independent variety in the concrete admixture, and the air entraining agent belongs to the admixture which needs to be mixed in the concrete construction technical specification. The air entraining agent is a surface active substance, can introduce a large amount of uniform and tiny air bubbles during the concrete mixing process, and the air bubbles are kept stable after the concrete is hardened.
The existing air entraining agents mainly comprise rosins and saponins air entraining agents, wherein the rosin air entraining agents take rosins as main raw materials and are combined with various chemical and physical modifications, so that the air entraining performance is good, but the problems of poor foaming performance, poor water solubility, difficulty in compounding with other additives and the like exist; the saponin air entraining agent is a macromolecular organic substance, has good foam stabilizing performance, but has the problem of high cost.
Through the above analysis, the problems and defects of the prior art are as follows: the existing air entraining agent has poor foaming performance and water solubility, is difficult to compound with other additives, and has higher cost.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a polyether air entraining agent, a preparation method and application.
The invention is realized in such a way that the preparation method of the polyether air entraining agent comprises the following steps:
screening the optimal ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer by using a single-factor experiment;
screening optimal preparation parameters, and weighing fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer according to the screened optimal proportion;
putting the weighed fatty alcohol-polyoxyethylene ether, sulfamic acid and catalyst into a flask under the condition of nitrogen protection, and stirring continuously;
and step four, heating the flask, reacting for a certain time at constant temperature, cooling, adding the modified silicone resin polyether microemulsion, and fully and uniformly stirring to obtain the polyether air entraining agent.
Further, the step one of screening the optimal mixture ratio of the fatty alcohol-polyoxyethylene ether, the sulfamic acid and the urea by using a single-factor experiment comprises the following steps:
determining experimental parameters by a single-factor variable method, determining the influence of the addition of sulfamic acid and urea on the molecular structure and yield of polyether, and screening to obtain the optimal ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid and urea.
Further, the step two of screening the optimal preparation parameters comprises the following steps:
determining the influence of the reaction time and temperature on the yield of polyether, testing the foaming performance of the product, and screening to obtain the optimal preparation parameters.
Further, the preparation method of the polyether air entraining agent also comprises the following steps:
and carrying out infrared characterization on the synthesized polyether air entraining agent, and determining a synthesis optimization scheme to further optimize the polyether air entraining agent.
Further, when the flask is heated in the fourth step, the temperature is gradually increased to 100-120 ℃, and the constant-temperature reaction time is 3.5-4 h.
And further, before adding the modified silicone polyether microemulsion in the fourth step, cooling to 60-70 ℃, adding 370 parts of hot water for dilution, and cooling to below 40 ℃.
The invention also aims to provide a polyether air entraining agent, which consists of 40 to 60 parts of fatty alcohol-polyoxyethylene ether, 15 to 25 parts of sulfamic acid, 0.3 to 1 part of catalyst and 8 to 15 parts of foam stabilizer by mass.
Further, the catalyst is urea, and the foam stabilizer is modified silicone polyether microemulsion.
The invention also aims to provide concrete added with the polyether air entraining agent.
In combination with the technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows:
the polyether air entraining agent prepared and synthesized by the invention has good air entraining effect, and the foaming performance test shows that the synthesized polyether air entraining agent has good foaming property.
According to the invention, the optimal ratio of the fatty alcohol-polyoxyethylene ether, the sulfamic acid, the catalyst and the foam stabilizer is screened through a single-factor experiment, so that the production cost can be effectively reduced, the prepared polyether air entraining agent has good foaming and foam stabilizing effects, and the loss of the air content of the concrete is remarkably reduced with time.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the high-performance concrete polyether air entraining agent prepared and synthesized by the invention can improve the workability and the homogeneity of concrete, improve the frost resistance of the concrete and greatly improve the comprehensive durability of the concrete.
Drawings
FIG. 1 is a flow chart of a preparation method of polyether air entraining agent provided by the embodiment of the invention;
FIG. 2 is a graph showing the effect of the admixture of the air entraining agent on the water reducing rate of concrete according to the embodiment of the invention;
FIG. 3 is a graph showing the influence of the admixture amount of the air entraining agent on the air content of the concrete provided by the embodiment of the invention;
FIG. 4 is a graph showing the effect of air content on water reducing rate of concrete according to an embodiment of the present invention;
fig. 5 is a graph of the compressive strength of concrete of 3, 7 and 28d age according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
1. Illustrative embodiments are explained. This section is an illustrative example developed to explain the claims in order to enable those skilled in the art to fully understand how to implement the present invention.
The polyether air entraining agent provided by the embodiment of the invention comprises 40-60 parts of fatty alcohol-polyoxyethylene ether, 15-25 parts of sulfamic acid, 0.3-1 part of catalyst and 8-15 parts of foam stabilizer by mass.
Preferably, the catalyst in the embodiment of the invention is urea, and the foam stabilizer is modified silicone polyether microemulsion.
As shown in fig. 1, a preparation method of a polyether air entraining agent provided by the embodiment of the present invention includes:
s101, screening the optimal mixture ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer by using a single-factor experiment;
s102, screening optimal preparation parameters, and weighing fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer according to the screened optimal proportion;
s103, putting the weighed fatty alcohol-polyoxyethylene ether, sulfamic acid and catalyst into a flask under the condition of nitrogen protection, and stirring continuously;
and S104, heating the flask, reacting at constant temperature for a certain time, cooling, adding the modified silicone resin polyether microemulsion, and fully and uniformly stirring to obtain the polyether air entraining agent.
The optimal proportion of the fatty alcohol-polyoxyethylene ether, the sulfamic acid and the urea screened by the single-factor experiment provided by the embodiment of the invention comprises the following components in parts by weight:
and determining experimental parameters by a single-factor variable method, determining the influence of the addition of sulfamic acid and urea on the molecular structure and yield of polyether, and screening to obtain the optimal mixture ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid and urea.
The screening of the optimal preparation parameters provided by the embodiment of the invention comprises the following steps:
determining the influence of the reaction time and temperature on the polyether yield, testing the foaming performance of the product, and screening to obtain the optimal preparation parameters.
The preparation method of the polyether air entraining agent provided by the embodiment of the invention also comprises the following steps:
and carrying out infrared characterization on the synthesized polyether air entraining agent, and determining a synthesis optimization scheme to further optimize the polyether air entraining agent.
In the embodiment of the invention, when the flask is heated in the step S104, the temperature is gradually increased to 100-120 ℃, and the constant-temperature reaction time is 3.5-4 h. Before adding the modified silicone polyether microemulsion, firstly cooling to 60-70 ℃, adding 370 parts of hot water for dilution, and then cooling to below 40 ℃.
2. Application examples. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is the application example of the technical scheme of the claims on specific products or related technologies.
The polyether air-entraining agent prepared by the embodiment of the invention can be applied to the preparation process of concrete, the performance of the concrete can be improved, and meanwhile, the concrete added with the polyether air-entraining agent can also be applied to road construction, bridge construction and other building construction.
3. Evidence of the relevant effects of the examples. The embodiment of the invention has some positive effects in the process of research and development or use, and indeed has great advantages compared with the prior art, and the following contents are described by combining data, charts and the like in the test process.
The preparation method of the concrete high-performance air entraining agent provided by the embodiment of the invention comprises the following steps:
(1) Synthesizing and characterizing a polyether air entraining agent;
(2) And (3) synthesizing and characterizing the hyperbranched rosin air entraining agent.
The screening method of the polyether air entraining agent provided by the embodiment of the invention comprises the following steps:
(1) A new experimental process is designed through a single-factor variable rule, the influence of the quantity of sulfamic acid and urea on the molecular structure and yield of polyether is researched, and the optimal raw material proportion of the process is screened out.
(2) The influence of the reaction time and temperature on the polyether yield is researched, the foaming performance of the product is tested, and the optimal reaction condition of the process is screened out.
(3) And performing infrared characterization on the synthetic sample, and further optimizing after determining a synthetic optimization scheme.
The embodiment of the invention synthesizes 9 polyether air-entraining agents, the infrared characterization of the polyether air-entraining agent synthesized by a small test shows that the structure of the polyether air-entraining agent is in accordance with the expected structure, the polyether air-entraining agent has good air-entraining effect, and meanwhile, the foaming performance test is preliminarily carried out to find that the synthesized sample has good foaming performance and is in accordance with the target requirement of the expected project.
Evaluation of concrete Properties:
the water reducing rate, the air content and the compressive strength ratio of the concrete added with the polyether air entraining agent (TEA) prepared by the embodiment of the invention are detected and compared with the AE sample of the air entraining agent, wherein the mixing amount of the TEA is (2-30) multiplied by 10 -5 The mixing amount of AE is (2-10) multiplied by 10 -5 2 × TEA represents TEA at 2 times the solids content, and the results are interpolated. The influence curve of the doping amount of the air entraining agent on the water reducing rate of the concrete is shown in figure 2; the influence curve of the air entraining agent dosage on the concrete air content is shown in figure 3; air content pairThe influence curve of the water reducing rate of the concrete is shown in figure 4; the influence curve of the air content on the compressive strength ratio of the concrete in the 3 rd, 7 th and 28 th ages is shown in figure 5.
The results in FIG. 2 show that the AE content is about 10X 10 when the water reducing rate of the concrete is about 6.0 percent -5 The amount of TEA added was about 12X 10 -5 (ii) a According to the analysis of the sensitivity of the water reducing rate of the concrete to the mixing amount of the air entraining agent, the sensitivity of AE is equivalent to that of TEA.
The results in FIG. 3 show that when the air content in the concrete is about 3.0%, the amount of TEA is (10-15). Times.10 -5 The content of AE is (5-10) x 10 -5 Within the range; according to the analysis of the sensitivity of the air content of the concrete to the mixing amount of the air entraining agent, the sensitivity of TEA is weaker.
FIG. 4 shows that when the water reducing rate of the concrete is about 6.0%, the air content of the concrete doped with AE is in the range of 3-4%, and the air content of the concrete doped with TEA is in the range of 2-3%, which indicates that the TEA has stronger dispersing effect under the same air content; according to the analysis of the sensitivity of the water reducing rate of the concrete to the air content, the TEA sensitivity is strong.
The results in FIG. 5 show that at 3d age, when the air content of the concrete is 3.0%, the compressive strength ratio of the concrete doped with TEA is above 95%, and the compressive strength ratio of the concrete doped with AE is less than 95%; when the concrete is at the age of 7d, the compressive strength ratio of the concrete doped with TEA and AE is more than 95%; during the 28d age, the doped TEA and AE are both more than 90%; under the condition of the same gas content, the compression strength ratio of the concrete doped with AE is relatively low in the ages of 3, 7 and 28d, which indicates that the AE introduces more bubbles in large size and the quality of the bubbles is not as good as that of TEA.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The preparation method of the polyether air entraining agent is characterized by comprising the following steps:
screening the optimal ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer by using a single-factor experiment;
screening optimal preparation parameters, and weighing fatty alcohol-polyoxyethylene ether, sulfamic acid, a catalyst and a foam stabilizer according to the screened optimal proportion;
putting the weighed fatty alcohol-polyoxyethylene ether, sulfamic acid and catalyst into a flask under the condition of nitrogen protection, and stirring continuously;
and step four, heating the flask, reacting for a certain time at constant temperature, cooling, adding the modified silicone resin polyether microemulsion, and fully and uniformly stirring to obtain the polyether air entraining agent.
2. The preparation method of the polyether air entraining agent according to claim 1, wherein the first step of screening the optimal mixture ratio of the fatty alcohol-polyoxyethylene ether, the sulfamic acid and the urea by using a one-factor experiment comprises the following steps:
determining experimental parameters by a single-factor variable method, determining the influence of the addition of sulfamic acid and urea on the molecular structure and yield of polyether, and screening to obtain the optimal ratio of fatty alcohol-polyoxyethylene ether, sulfamic acid and urea.
3. The method for preparing the polyether air entraining agent according to claim 1, wherein the step two of screening the optimal preparation parameters comprises the following steps:
determining the influence of the reaction time and temperature on the polyether yield, testing the foaming performance of the product, and screening to obtain the optimal preparation parameters.
4. The method for preparing the polyether air entraining agent according to claim 1, further comprising:
and carrying out infrared characterization on the synthesized polyether air entraining agent, and determining a synthesis optimization scheme to further optimize the polyether air entraining agent.
5. The preparation method of the polyether air entraining agent according to the claim 1, wherein the flask is heated in the fourth step, the temperature is gradually increased to 100-120 ℃, and the constant temperature reaction time is 3.5-4 h.
6. The preparation method of the polyether air entraining agent according to claim 1, wherein before the modified silicone polyether microemulsion is added in the fourth step, the temperature is reduced to 60-70 ℃, 370 parts of hot water is added for dilution, and then the temperature is reduced to below 40 ℃.
7. The polyether air-entraining agent prepared by the preparation method of the polyether air-entraining agent disclosed by any one of claims 1 to 6 is characterized by comprising 40-60 parts of fatty alcohol-polyoxyethylene ether, 15-25 parts of sulfamic acid, 0.3-1 part of catalyst and 8-15 parts of foam stabilizer in parts by mass.
8. The polyether air entraining agent of claim 7 wherein the catalyst is urea and the foam stabilizer is a modified silicone polyether microemulsion.
9. Concrete to which the polyether air-entraining agent according to any one of claims 7 to 8 is added.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018086610A1 (en) * | 2016-11-14 | 2018-05-17 | 清华大学 | Polymer and preparation method and application thereof |
| CN109279809A (en) * | 2018-09-30 | 2019-01-29 | 贵州凯襄新材料有限公司 | A kind of modified air entraining agent and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018086610A1 (en) * | 2016-11-14 | 2018-05-17 | 清华大学 | Polymer and preparation method and application thereof |
| CN109279809A (en) * | 2018-09-30 | 2019-01-29 | 贵州凯襄新材料有限公司 | A kind of modified air entraining agent and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 唐修生;方绪顺;温金保;刘兴荣;黄国泓;祝烨然;: "聚醚类引气剂的制备及其应用性能评价", 混凝土, no. 04, 27 April 2016 (2016-04-27), pages 76 * |
| 唐修生;林宇辉;温金保;黄国泓;祝烨然;: "聚醚类引气剂的合成研究", 新型建筑材料, no. 11, 25 November 2016 (2016-11-25) * |
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