CN106746870A - It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing - Google Patents
It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing Download PDFInfo
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- CN106746870A CN106746870A CN201510808231.XA CN201510808231A CN106746870A CN 106746870 A CN106746870 A CN 106746870A CN 201510808231 A CN201510808231 A CN 201510808231A CN 106746870 A CN106746870 A CN 106746870A
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- Prior art keywords
- water
- collapsing
- sustained
- reactor
- agent
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- 238000013268 sustained release Methods 0.000 title claims abstract description 28
- 239000012730 sustained-release form Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 12
- 125000001844 prenyl group Chemical group [H]C([*])([H])C([H])=C(C([H])([H])[H])C([H])([H])[H] 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 8
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 8
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000176 sodium gluconate Substances 0.000 claims abstract description 8
- 229940005574 sodium gluconate Drugs 0.000 claims abstract description 8
- 235000012207 sodium gluconate Nutrition 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 description 19
- 229920005646 polycarboxylate Polymers 0.000 description 14
- 238000012360 testing method Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 7
- 239000004568 cement Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 229920013730 reactive polymer Polymers 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
Present invention offer is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing, and is related to technical field of concrete additives, and it is comprised the following steps：The first step, by prenyl polyoxyethylene ether 7%, maleic anhydride 5.5%, acryloyl ammonium 16%, ammonium persulfate 18%, NaOH 3.7%, sodium gluconate 12%, be ready to for each component by the weight proportion of balance of water, a part of water is taken to add in reactor and the water in reactor is heated into 52-55 DEG C, then while stirring, while toward adding prenyl polyoxyethylene ether in reactor；Second step, after prenyl polyoxyethylene ether is completely dissolved, then toward maleic anhydride, acryloyl ammonium, ammonium persulfate is sequentially added in reactor, is then heated to 72-74 DEG C by solution, continuously stirs 3.5 hours；3rd step, sequentially adds NaOH, sodium gluconate, then continuously stirs 1 hour, finally adds and can obtain the sustained-release polycarboxylic into remaining water and protect agent of collapsing；Above steps is to carry out at ambient pressure.
Description
Technical field
It is more particularly to a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing the present invention relates to technical field of concrete additives.
Background technology
Guarantor's agent of collapsing is the additive that can keep slump not immediate loss, and guarantor's agent of collapsing mainly rises and delays hydrated cementitious to condense, and reaches the effect for keeping slump.
Most common problem is too fast loss of slump in cement adaptability.The method for being used for reducing polycarboxylate water-reducer loss of slump at present mainly has 5 kinds：（1）Compound slow setting component；（2）The repeated multiple times addition of water reducer；（3）Additive process after water reducer；（4）Sustained release method；（5）Compounding reactive polymer copolymer.
In too fast this problem for loss of slump, additive worker generally improves the guarantor of water reducer and collapses ability with polycarboxylate water-reducer and retarder compounding.It is particularly problematic particularly when transportation range is more long but above-mentioned way far can not meet requirement of engineering.The addition of retarder can not fundamentally solve the problems, such as that existing polycarboxylate water-reducer is protected and collapse that ability is weak, and excessive incorporations retarder can be such that the setting time of concrete extend on the contrary, reduction concrete quality, influence construction speed.Then, exploitation one kind can keep slump not lose in a long time, and not influence the guarantor of maturing later stage performance to collapse agent just into the study hotspot of concrete admixture.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of sustained-release polycarboxylic for preparing and protects the method for agent of collapsing, the sustained-release polycarboxylic prepared by the method protects agent of collapsing can keep slump not lose in a long time, and not influence the guarantor of maturing later stage performance to collapse agent.
In order to solve the above-mentioned technical problem, the present invention is adopted the following technical scheme that：It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing, comprise the following steps：
The first step, according to prenyl polyoxyethylene ether 7%, maleic anhydride 5.5%, acryloyl ammonium 16%, ammonium persulfate 18%, NaOH 3.7%, sodium gluconate 12%, be ready to for each component by the weight proportion of balance of water, and be contained in container each component respectively, a part of water is taken from the container of dress water to add in reactor and the water in reactor is heated into 52-55 DEG C, then while stirring, while toward adding prenyl polyoxyethylene ether in reactor；
Second step, after prenyl polyoxyethylene ether is completely dissolved, then toward maleic anhydride, acryloyl ammonium, ammonium persulfate is sequentially added in reactor, is then heated to 72-74 DEG C by solution, continuously stirs 3.5 hours；
3rd step, sequentially adds NaOH, sodium gluconate, then continuously stirs 1 hour, finally adds and can obtain the sustained-release polycarboxylic into remaining water and protect agent of collapsing；
Above steps is to carry out at ambient pressure.
The present invention obtain beneficial effect be：Sustained-release polycarboxylic prepared by the method provided by the present invention protects agent of collapsing and overcomes the excessive too fast shortcoming of existing polycarboxylate water-reducer loss of slump with polycarboxylate water-reducer compound use, guarantor's effect of collapsing is obvious, simultaneously, it can keep the mobility of fresh concrete, for the use of concrete creates favourable condition, in addition, the sustained-release polycarboxylic protects collapse agent and polycarboxylate water-reducer compound use, due to the raising of water-reducing rate, the intensity of concrete increased, and also overcome the low shortcoming of early age strength of concrete.
Specific embodiment
It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing as one embodiment of the present invention, comprise the following steps：
The first step, according to prenyl polyoxyethylene ether 7%, maleic anhydride 5.5%, acryloyl ammonium 16%, ammonium persulfate 18%, NaOH 3.7%, sodium gluconate 12%, be ready to for each component by the weight proportion of balance of water, and be contained in container each component respectively, a part of water is taken from the container of dress water to add in reactor and the water in reactor is heated into 52-55 DEG C, then while stirring, while toward adding prenyl polyoxyethylene ether in reactor；
Second step, after prenyl polyoxyethylene ether is completely dissolved, then toward maleic anhydride, acryloyl ammonium, ammonium persulfate is sequentially added in reactor, is then heated to 72-74 DEG C by solution, continuously stirs 3.5 hours；
3rd step, sequentially adds NaOH, sodium gluconate, then continuously stirs 1 hour, finally adds and can obtain the sustained-release polycarboxylic into remaining water and protect agent of collapsing；
Above steps is to carry out at ambient pressure.
Sustained-release polycarboxylic being prepared according to said ratio and preparation method and protecting agent of collapsing, hereafter, agent of collapsing is protected with the sustained-release polycarboxylic for obtaining carries out paste flowing degree test, and paste flowing degree test is with reference to GB/T8077-2000《Concrete admixture homogeneity test method》In flowing degree of net paste of cement method of testing carry out, finally measure and filled guarantor and collapse after agent, flowing degree of net paste of cement is lost 5% or so with the extension of time, illustrate that guarantor's agent of collapsing is highly beneficial to reduction fluidity loss.
Then the sustained-release polycarboxylic that will be obtained protects agent of collapsing and the test of water-reducing rate, loss of slump, concrete crushing strength is carried out by following concrete mix, and test result is as described below.
Concrete each component weight proportion：The weight portion of cement 32, the weight portion of river sand 73, the weight portion of handstone 33 of 0.3-0.8 centimetres of diameter, the weight portion of middle stone 44 of 1-1.5 centimetres of diameter, the weight portion of big stone 33 of 1.8-2.4 centimetres of diameter.
In water-reducing rate, loss of slump, the test of concrete crushing strength, the adding proportion of polycarboxylate water-reducer is 0.7%（Weight ratio）, the adding proportion that sustained-release polycarboxylic protects agent of collapsing is 0.1%（Weight ratio）.
Water-reducing rate test result is：In the case of the polycarboxylate water-reducer of simple addition 0.7%, water-reducing rate is 26.5%, and in the case where the sustained-release polycarboxylic of simple addition 0.1% protects agent of collapsing, water-reducing rate is 13%, after compound addition polycarboxylate water-reducer and sustained-release polycarboxylic protect agent of collapsing, water-reducing rate is 35%.Can be seen that guarantor agent of collapsing by above-mentioned test result has certain water-reducing effect, after it is compound with polycarboxylate water-reducer, with cooperative effect, the water-reduction of water reducer is substantially increased, the raising of this water-reducing rate will be significant to saving cement and raising concrete strength.
Loss of slump test result is：In the case of the polycarboxylate water-reducer of simple addition 0.7%, initial slump degree is 235 millimeters, it is 215 millimeters after 60 minutes, it is 190 millimeters after 90 minutes, after compound addition polycarboxylate water-reducer and sustained-release polycarboxylic protect agent of collapsing, initial slump degree is 250 millimeters, is 240 millimeters after 60 minutes, is 230 millimeters after 90 minutes.It can thus be seen that be not added with the sustained-release polycarboxylic protect collapse agent when, slump loss it is larger, just have lost within 60 minutes 20 millimeters, after 90 minutes be even more loss reach 45 millimeters；After addition sustained-release polycarboxylic protects agent of collapsing, slump loss is smaller, and 20 millimeters are only have lost after 90 minutes, it was demonstrated that the sustained-release polycarboxylic protects agent of collapsing and overcomes the excessive too fast shortcoming of existing polycarboxylate water-reducer loss of slump, protects effect of collapsing obvious.
Concrete crushing strength experiment is with reference to GB8076-2008《Concrete admixture》, experiment concrete match ratio ratio of mud W/C=0.29,20 DEG C of experimental temperature.Concrete crushing strength test result is：In the case of the polycarboxylate water-reducer of simple addition 0.7%, concrete 3d intensity is 35.3 MPas, 43.6 MPas of 7d intensity, 59.7 MPas of 28d intensity, after compound addition sustained-release polycarboxylic protects agent of collapsing, concrete 3d intensity is 38.5 MPas, 46.4 MPas of 7d intensity, 62.3 MPas of 28d intensity.It is possible thereby to determine, the sustained-release polycarboxylic is protected agent of collapsing and is used with polycarboxylic acids water reducing agent compositional, and because water-reducing rate is improved, the intensity of concrete increased, while overcoming the low shortcoming of early age strength of concrete.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner, and any obvious replacement is within protection scope of the present invention on the premise of the technical program design is not departed from.
Finally, it should be emphasized that, in order to allow those of ordinary skill in the art more easily to understand improvements of the present invention relative to prior art, some descriptions of the invention have been simplified, and for the sake of clarity, present specification is omitted some other elements, and those of ordinary skill in the art should be aware that these elements for omitting also may make up present disclosure.
Claims (1)
1. it is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing, comprise the following steps：
The first step, according to prenyl polyoxyethylene ether 7%, maleic anhydride 5.5%, acryloyl ammonium 16%, ammonium persulfate 18%, NaOH 3.7%, sodium gluconate 12%, be ready to for each component by the weight proportion of balance of water, and be contained in container each component respectively, a part of water is taken from the container of dress water to add in reactor and the water in reactor is heated into 52-55 DEG C, then while stirring, while toward adding prenyl polyoxyethylene ether in reactor；
Second step, after prenyl polyoxyethylene ether is completely dissolved, then toward maleic anhydride, acryloyl ammonium, ammonium persulfate is sequentially added in reactor, is then heated to 72-74 DEG C by solution, continuously stirs 3.5 hours；
3rd step, sequentially adds NaOH, sodium gluconate, then continuously stirs 1 hour, finally adds and can obtain the sustained-release polycarboxylic into remaining water and protect agent of collapsing；
Above steps is to carry out at ambient pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510808231.XA CN106746870A (en) | 2015-11-20 | 2015-11-20 | It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510808231.XA CN106746870A (en) | 2015-11-20 | 2015-11-20 | It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing |
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| Publication Number | Publication Date |
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| CN106746870A true CN106746870A (en) | 2017-05-31 |
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| CN201510808231.XA Pending CN106746870A (en) | 2015-11-20 | 2015-11-20 | It is a kind of to prepare the method that sustained-release polycarboxylic protects agent of collapsing |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0995728A1 (en) * | 1998-10-23 | 2000-04-26 | Nissan Chemical Industries, Ltd. | Process for preparing an aqueous solution of sulfanilic acid modified melamine-formaldehyde resin and a cement composition |
| CN102504126A (en) * | 2011-11-03 | 2012-06-20 | 山西合盛邦砼建材有限公司 | Slump loss resistant type gather carboxylate water-reducing agent and preparation method thereof |
| CN103755208A (en) * | 2013-12-19 | 2014-04-30 | 柳州正菱集团有限公司 | Concrete slump retaining agent |
-
2015
- 2015-11-20 CN CN201510808231.XA patent/CN106746870A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0995728A1 (en) * | 1998-10-23 | 2000-04-26 | Nissan Chemical Industries, Ltd. | Process for preparing an aqueous solution of sulfanilic acid modified melamine-formaldehyde resin and a cement composition |
| CN102504126A (en) * | 2011-11-03 | 2012-06-20 | 山西合盛邦砼建材有限公司 | Slump loss resistant type gather carboxylate water-reducing agent and preparation method thereof |
| CN103755208A (en) * | 2013-12-19 | 2014-04-30 | 柳州正菱集团有限公司 | Concrete slump retaining agent |
Non-Patent Citations (2)
| Title |
|---|
| 何廷树等: "《土木工程材料》", 31 January 2013, 中国建材工业出版社 * |
| 刘春燕: "保坍型聚羧酸减水剂的合成及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
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Application publication date: 20170531 |
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