CN102911323A - Low-temperature synthetic method of high-performance polycarboxylic acid water reducing agent - Google Patents
Low-temperature synthetic method of high-performance polycarboxylic acid water reducing agent Download PDFInfo
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- CN102911323A CN102911323A CN2012104302637A CN201210430263A CN102911323A CN 102911323 A CN102911323 A CN 102911323A CN 2012104302637 A CN2012104302637 A CN 2012104302637A CN 201210430263 A CN201210430263 A CN 201210430263A CN 102911323 A CN102911323 A CN 102911323A
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Abstract
The invention discloses a synthetic method of a polycarboxylic acid water reducing agent. The method includes preparing a solution A and a solution B according to a mass ratio, dropwise adding the A solution and the B solution to a reactor with deionized water and allyl alcohol polyoxyethylene ether which are prepared according to a mass ratio for 3-3.5 hours, reacting the mixture under the temperature of 55-60 DEG C, continuing reaction for 1-1.5 hours after adding, lowering the temperature to 50 DEG C, and using a sodium hydroxide solution to neutralize the mixture until potential of hydrogen (PH) reaches 6-7 to obtain the object product. According to the synthetic method, the operation is convenient, the reaction process is easy to control, production efficiencies are improved, and production costs are reduced to a certain extent; the produced water reducing agent is good in adaptability and basically adaptive to all kinds of cement; the water reducing rate of the water reducing agent is high and reaches over 30%; and the admixture amount is small, the dosage of the agent converted into the solid is 0.1%-0.25%, and strength of concrete at each age is obviously improved.
Description
Technical field
The present invention relates to a kind of synthetic method of water reducer, particularly under lower temperature conditions, synthesize the method for high performance water reducing agent of polyocarboxy acid.
Background technology
Water reducer can effectively improve concrete workability, improves concrete intensity, prolongs concrete weather resistance.Concentrate in stirring, mechanical transportation and the pumping construction process at the concrete that current level of automation is higher, water reducer plays an important role, and has become indispensable component in the concrete.
According to the evolution of water reducer, generally the development of water reducer is divided into three phases: the first-generation is the ordinary water-reducing agent take wooden calcium, wooden sodium as representative, and water-reducing rate is 6%～12%; The s-generation is the high efficiency water reducing agent take naphthalene system and trimeric cyanamide as representative, and there are the problems such as formaldehyde pollution in water-reducing rate 15%～25% in production and use procedure; The third generation is the high-performance water reducing agent take polycarboxylate as representative, has water-reducing rate high (can reach 30%), volume few (0.2%～0.4%), institute's concrete batching has the advantages such as intensity is high, environmental protection, is leading product and the developing direction of from now on admixture industry.
The approach of macromolecular synthetic reaction is a lot, can be divided into copolymerization, addition polymerization, polycondensation etc. according to reaction mechanism.High performance water reducing agent of polyocarboxy acid mainly be by unsaturated monomer under the effect of initiator, will be grafted on the main chain of polymkeric substance with the active group of side chain, thereby obtain polycarboxylate water-reducer molecule with pectination.At present, the synthesis temperature of polycarboxylate water-reducer is mostly at 80～120 ℃, and the reaction times is 3～8h.
Therefore, by adopting more scientific rational method, utilize more efficient synthetic method, further improve the production efficiency of polycarboxylate water-reducer, reduce production costs, for further applying of polycarboxylate water-reducer, have important economic benefit and social benefit.
Summary of the invention
In order to overcome above-mentioned deficiency of the prior art, the invention provides provides a kind of more efficiently synthetic method of polycarboxylate water-reducer, produce according to present method, temperature of reaction is low can hang down to 60 ℃), reaction times is as short as 3h, therefore, production efficiency is higher, and production cost also has certain reduction.The water reducer adaptability of producing is good, substantially adapts to all kinds of cement; Water-reducing rate is high, and its water-reducing rate is greater than 30%; Volume is few, and the solid volume of folding is 0.1%～0.25%, and the concrete strength in each age phase also obviously improves.
The object of the present invention is achieved like this:
A kind of low-temperature synthetic method of high performance water reducing agent of polyocarboxy acid, its preparation method is as follows:
The preparation of the first step, A liquid: respectively take by weighing vinylformic acid and deionized water at 18: 12 with mass ratio, stir, evenly rear stand-by;
The preparation of second step, B liquid: respectively take by weighing deionized water, Thioglycolic acid, methylpropene sodium sulfonate at 56: 0.375: 2.8 with mass ratio and carry out mix and blend, until stand-by behind the homogeneous transparent;
The 3rd the step, respectively take by weighing deionized water and allyl alcohol polyethenoxy ether at 200: 183 with mass ratio, join in the reactor, and stir and be warmed up to 55～60 ℃, add 0.5% ammonium persulfate initiator of large monomer mass until temperature after steadily, stir, keep temperature-stable;
After the 4th step, the first step to the three go on foot and finish, drip A liquid and B liquid in the reactor during beginning goes on foot to the 3rd, temperature of reaction is controlled at 55～60 ℃, time for adding is 3～3.5h, dropwise, continue reaction 1～1.5h, be cooled to 50 ℃, being neutralized to PH with sodium hydroxide solution is 6～7, obtains target product.
Positive beneficial effect:The present invention carries out the synthetic of polycarboxylate water-reducer, can effectively reduce temperature of reaction, Reaction time shorten, and easy and simple to handle, reaction process is easier to control, and production efficiency improves high, and production cost also has certain reduction; The water reducer adaptability of producing is good, substantially adapts to all kinds of cement; Water-reducing rate is high, and its water-reducing rate is greater than 30%; Volume is few, and the solid volume of folding is 0.1%～0.25%, and the concrete strength in each age phase also obviously improves.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described:
A kind of low-temperature synthetic method of high performance water reducing agent of polyocarboxy acid, its preparation method is as follows:
The preparation of the first step, A liquid: respectively take by weighing vinylformic acid and deionized water at 18: 12 with mass ratio, stir, evenly rear stand-by;
The preparation of second step, B liquid: respectively take by weighing deionized water, Thioglycolic acid, methylpropene sodium sulfonate at 56: 0.375: 2.8 with mass ratio and carry out mix and blend, until stand-by behind the homogeneous transparent;
The 3rd the step, respectively take by weighing deionized water and allyl alcohol polyethenoxy ether at 200: 183 with mass ratio, join in the reactor, and stir and be warmed up to 55～60 ℃, add 0.5% ammonium persulfate initiator of large monomer mass until temperature after steadily, stir, keep temperature-stable;
After the 4th step, the first step to the three go on foot and finish, drip A liquid and B liquid in the reactor during beginning goes on foot to the 3rd, temperature of reaction is controlled at 55～60 ℃, time for adding is 3～3.5h, dropwise, continue reaction 1～1.5h, be cooled to 50 ℃, being neutralized to PH with sodium hydroxide solution is 6～7, obtains target product.
Only starch the contrast experiment for above-mentioned synthetic polycarboxylate water-reducer and domestic and international product, this experiment cement adopts Xiaoshan Mountain PO42.5R cement 300g, water 87g, concrete experimental result such as following table:
As can be seen from the above table, polycarboxylate water-reducer of the present invention has preferably water-reducing effect, higher dispersive ability, little through time loss, effect and external product are suitable, and production process is easier, be more prone to control, save energy consumes, and has reduced production cost, is conducive to applying of polycarboxylate water-reducer.
Above embodiment only is used for illustrating preferred implementation of the present invention; but the present invention is not limited to above-mentioned embodiment; in the ken that described field those of ordinary skill possesses; any modification of doing within the spirit and principles in the present invention, be equal to and substitute and improvement etc., it all should be encompassed within the technical scheme scope that the present invention asks for protection.
Claims (1)
1. the low-temperature synthetic method of a high performance water reducing agent of polyocarboxy acid is characterized in that its preparation method, and concrete steps are as follows:
The preparation of the first step, A liquid: respectively take by weighing vinylformic acid and deionized water at 18: 12 with mass ratio, stir, evenly rear stand-by;
The preparation of second step, B liquid: respectively take by weighing deionized water, Thioglycolic acid, methylpropene sodium sulfonate at 56: 0.375: 2.8 with mass ratio and carry out mix and blend, until stand-by behind the homogeneous transparent;
The 3rd the step, respectively take by weighing deionized water and allyl alcohol polyethenoxy ether at 200: 183 with mass ratio, join in the reactor, and stir and be warmed up to 55～60 ℃, add 0.5% ammonium persulfate initiator of large monomer mass until temperature after steadily, stir, keep temperature-stable;
After the 4th step, the first step to the three go on foot and finish, drip A liquid and B liquid in the reactor during beginning goes on foot to the 3rd, temperature of reaction is controlled at 55～60 ℃, time for adding is 3～3.5h, dropwise, continue reaction 1～1.5h, be cooled to 50 ℃, being neutralized to PH with sodium hydroxide solution is 6～7, obtains target product.
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| CN201210430263.7A CN102911323B (en) | 2012-11-01 | 2012-11-01 | A kind of low-temperature synthetic method of high performance water reducing agent of polyocarboxy acid |
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| CN201210430263.7A CN102911323B (en) | 2012-11-01 | 2012-11-01 | A kind of low-temperature synthetic method of high performance water reducing agent of polyocarboxy acid |
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| CN102911323A true CN102911323A (en) | 2013-02-06 |
| CN102911323B CN102911323B (en) | 2016-06-08 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110065847A1 (en) * | 2008-05-14 | 2011-03-17 | Nippon Shokubai Co., Ltd. | Method for producing polycarboxylic acid copolymer and copolymer composition for cement admixture |
| CN102515618A (en) * | 2011-11-30 | 2012-06-27 | 上海大学 | Slow release slump retaining polycarboxylate water reducer and preparation thereof |
| CN102718426A (en) * | 2012-06-21 | 2012-10-10 | 马清浩 | Modified carboxylic acid water-reducing agent and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110065847A1 (en) * | 2008-05-14 | 2011-03-17 | Nippon Shokubai Co., Ltd. | Method for producing polycarboxylic acid copolymer and copolymer composition for cement admixture |
| CN102515618A (en) * | 2011-11-30 | 2012-06-27 | 上海大学 | Slow release slump retaining polycarboxylate water reducer and preparation thereof |
| CN102718426A (en) * | 2012-06-21 | 2012-10-10 | 马清浩 | Modified carboxylic acid water-reducing agent and preparation method thereof |
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