CN103923276A - Method for synthesizing polyether-type polycarboxylate water reducer - Google Patents
Method for synthesizing polyether-type polycarboxylate water reducer Download PDFInfo
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- CN103923276A CN103923276A CN201410173879.XA CN201410173879A CN103923276A CN 103923276 A CN103923276 A CN 103923276A CN 201410173879 A CN201410173879 A CN 201410173879A CN 103923276 A CN103923276 A CN 103923276A
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- water reducer
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Abstract
The invention discloses a method for synthesizing a polyether-type polycarboxylate water reducer. The method comprises the following steps: adding ammonium persulfate as an initiator after dissolving isoamylene polyethylene glycol propyl ether, a crylic acid, sodium methallyl sulfonate, 2-acrylamide-2-methyl propane sulfonic acid and water; cooling after reacting at 70 DEG C for 7 hours; and neutralizing by using sodium hydroxide until the pH is 6-7, and then compounding a little of sodium gluconate to discharge. The water reducer obtained by the method has high water reducing rate and good slump retaining performance, and is especially suitable for preparation of high-grade and early strength concrete, and the strength of the obtained concrete mixture can be greatly improved.
Description
Technical field
The invention belongs to cement additire field, be specifically related to a kind of synthetic method of polyether-type poly carboxylic acid series water reducer.
Background technology
Water reducer is a kind of requisite component in high performance concrete.Polycarboxylate high performance water-reducing agent is because structure easily regulates and controls, and polymerization is easy, in the research of water reducer, occupies critical role.At present, domestic polycarboxylic acids dehydragent mainly contains following two types: polyester and polyethers.Comparatively speaking, the preparation were established of polyester water reducer is long, critical control point is many, solvent during esterification needs to reclaim, production cost is higher, and the synthesis technique of polyethers water reducer is simple, production technique environmental protection, polymerization concentration is high, shelf lives is long, preparation cost is low, therefore, the research of polyethers water reducer and application are more and more subject to people's concern (Yuan LD, Ding JH, Chen JW, Investigation on the synthesis conditions of ether polycarboxylic acid-type water-reducing agents by means of GPC, Concrete, 2012, 4).
On Vehicles Collected from Market, the polyethers water reducer of main flow mostly is the Binary Aggregation system of vinylformic acid and polyoxyethylene glycol allyl ethers (or polyoxyethylene glycol isopentene propyl ether), and the unsaturated sulfonic acid monomers such as methylpropene sodium sulfonate that add that have form ternary copolymerization system to promote its water-reducing property.But because the large monomer of polyethers has stronger chain transfer, not only make the molecular weight of product lower, molecular weight distribution broadens, and cause making in water reducer molecule the molar fraction of the long side chain of polyoxyethylene and sulfonic acid group on the low side, thereby cause that its water reducing ability compares obvious reduction with slump retaining with polyester water reducer.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of synthetic method with the polyether-type poly carboxylic acid series water reducer of high water reducing rate.
The technical solution used in the present invention is:
Use quaternary monomer copolymerization system, monomer comprises polyoxyethylene glycol isopentene propyl ether, vinylformic acid, methylpropene sodium sulfonate and 2-acrylamide-2-methylpro panesulfonic acid, their mol ratio is 1:6:0.8:0.3, after four kinds of monomers and water are dissolved each other, form reaction system, in reaction system, drip initiator ammonium persulfate solution, under stirring, in 7 hours 70 oC reaction times;
After reaction finishes, reaction system is down to room temperature, regulates the pH to 6-7 of reaction system, and add the Sunmorl N 60S that accounts for water reducer total mass 4%-5%, obtain polyether-type poly carboxylic acid series water reducer.
Polyether-type poly carboxylic acid series water reducer prepared by the inventive method can be directly used in preparation high performance concrete.
Polyoxyethylene glycol isopentene propyl ether molecular weight used is 2400 ~ 2600.
Ammonium persulphate consumption is 4% ~ 6% of reaction monomers total mass.
Compared with prior art, the beneficial effect of the inventive method:
Preparation method's technological process of the present invention is simple, without waste material, produce, and the water reducer obtaining has very high water reducing ability and good function of slump protection, and can significantly improve the intensity of gained concrete mix, its correlated performance index surpasses the technical requirements of retardation setting type acceptable end product high performance water reducing agent of polyocarboxy acid of JG/T 223-2007 < < polycarboxylate high performance water-reducing agent > > regulation and the technical requirements of the retardation setting type high-performance water reducing agent of GB/T 8076-2008 < < concrete admixture > > regulation.Be particularly suitable for preparing high grade and early strength concrete.
Accompanying drawing explanation
Fig. 1 is that the inventive method is at the reaction unit of laboratory small-scale operations.
Embodiment
Below by embodiment, introduce in detail the present invention, the reagent adopting is the general industry level reagent of buying on the market, and the inventive method is shown in Fig. 1 at the reaction unit of laboratory small-scale operations.
Embodiment 1
Take polyoxyethylene glycol isopentene propyl ether 60.00g, vinylformic acid 10.81g, 2-acrylamide-2-methylpro panesulfonic acid 3.11 g, methylpropene sodium sulfonate 6.32 g, distilled water 108g is in the device shown in Fig. 1.Under agitation mixture is warming up to 70oC, at the uniform velocity drip 3.20g ammonium persulphate and be dissolved in the solution that 80g distilled water forms, in 3 hours, dropwise, isothermal reaction 4 hours more subsequently, after cooling, with the pH to 6-7 of sodium hydroxide solution regulation system, and add 10.7g Sunmorl N 60S, get final product to such an extent that can be directly used in the efficient polycarboxylate water-reducer of preparing high performance concrete.
Embodiment 2:
Take polyoxyethylene glycol isopentene propyl ether 60.00 g, vinylformic acid 10.81g, 2-acrylamide-2-methylpro panesulfonic acid 3.11 g, methylpropene sodium sulfonate 6.32 g are in the device shown in Fig. 1.Distilled water 108g is in the device shown in Fig. 1.Under agitation mixture is warming up to 70oC, at the uniform velocity drip 4.81g ammonium persulphate and be dissolved in the solution that 80g distilled water forms, in 3 hours, dropwise, isothermal reaction 4 hours more subsequently, after cooling, with the pH to 6-7 of sodium hydroxide solution regulation system, and add 13.4g Sunmorl N 60S, get final product to such an extent that can be directly used in the efficient polycarboxylate water-reducer of preparing high performance concrete.
Obtained polycarboxylate water-reducer is according to GB/T 8077-2000 < < Methods for testing uniformity of concrete admixture > > test, and detailed performance is relatively in Table 1.
Table 1 the inventive method gained polycarboxylate water-reducer performance and and standard comparison
Its correlated performance index of the obtained polycarboxylate water-reducer of the inventive method surpasses the technical requirements of retardation setting type acceptable end product high performance water reducing agent of polyocarboxy acid of JG/T 223-2007 < < polycarboxylate high performance water-reducing agent > > regulation and the technical requirements of the retardation setting type high-performance water reducing agent of GB/T 8076-2008 < < concrete admixture > > regulation.
Claims (3)
1. a synthetic method for polyether-type poly carboxylic acid series water reducer, is characterized in that:
Use quaternary monomer copolymerization system, monomer comprises polyoxyethylene glycol isopentene propyl ether, vinylformic acid, methylpropene sodium sulfonate and 2-acrylamide-2-methylpro panesulfonic acid, their mol ratio is 1:6:0.8:0.3, after four kinds of monomers and water are dissolved each other, form reaction system, in reaction system, drip initiator ammonium persulfate solution, under stirring, in 7 hours 70 oC reaction times;
After reaction finishes, reaction system is down to room temperature, regulates the pH to 6-7 of reaction system, and add the Sunmorl N 60S that accounts for water reducer total mass 4%-5%, obtain polyether-type poly carboxylic acid series water reducer.
2. the synthetic method of polyether-type poly carboxylic acid series water reducer as claimed in claim 1, is characterized in that: preparing water reducer polyoxyethylene glycol isopentene propyl ether molecular weight used is 2400 ~ 2600.
3. the synthetic method of polyether-type poly carboxylic acid series water reducer as claimed in claim 1, is characterized in that: ammonium persulphate consumption is 4% ~ 6% of reaction monomers total mass.
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| CN201410173879.XA CN103923276A (en) | 2014-04-28 | 2014-04-28 | Method for synthesizing polyether-type polycarboxylate water reducer |
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| CN201410173879.XA CN103923276A (en) | 2014-04-28 | 2014-04-28 | Method for synthesizing polyether-type polycarboxylate water reducer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106632891A (en) * | 2016-12-27 | 2017-05-10 | 陕西友邦新材料科技有限公司 | Polycarboxylate superplasticizer mother solution based on steam-cured concrete and preparation method of polycarboxylate superplasticizer mother solution |
| CN106749955A (en) * | 2015-11-20 | 2017-05-31 | 衡阳市银利实业有限公司 | A kind of anti-chamotte mould polycarboxylate water-reducer |
| CN106750045A (en) * | 2015-11-20 | 2017-05-31 | 衡阳市银利实业有限公司 | A kind of method for preparing anti-chamotte mould polycarboxylate water-reducer |
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| CN101817657A (en) * | 2009-02-26 | 2010-09-01 | 北京东方雨虹防水技术股份有限公司 | Polycarboxylic acid slump retaining agent |
| CN102173639A (en) * | 2011-01-27 | 2011-09-07 | 南京瑞迪高新技术公司 | Polycarboxylate-based water-reducing agent with effect of inhibiting corrosion of steel bars and preparation method thereof |
| CN102344535A (en) * | 2011-08-02 | 2012-02-08 | 武汉市奥维邦科技发展有限公司 | Preparation method of modified high-performance polycarboxylic acid water reducing agent |
| CN102503226A (en) * | 2011-10-19 | 2012-06-20 | 中建商品混凝土有限公司 | High slump retaining type polycarboxylic acid water reducing agent with sustained-release effect and preparation method thereof |
| CN102911320A (en) * | 2012-07-21 | 2013-02-06 | 北京工业大学 | Method for preparing powder polycarboxylic acid superplasticizer |
| CN103373832A (en) * | 2012-04-17 | 2013-10-30 | 苏琳 | High-performance anti-cracking anticorrosive water reducing agent composition and preparation method thereof |
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2014
- 2014-04-28 CN CN201410173879.XA patent/CN103923276A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101817657A (en) * | 2009-02-26 | 2010-09-01 | 北京东方雨虹防水技术股份有限公司 | Polycarboxylic acid slump retaining agent |
| CN102173639A (en) * | 2011-01-27 | 2011-09-07 | 南京瑞迪高新技术公司 | Polycarboxylate-based water-reducing agent with effect of inhibiting corrosion of steel bars and preparation method thereof |
| CN102344535A (en) * | 2011-08-02 | 2012-02-08 | 武汉市奥维邦科技发展有限公司 | Preparation method of modified high-performance polycarboxylic acid water reducing agent |
| CN102503226A (en) * | 2011-10-19 | 2012-06-20 | 中建商品混凝土有限公司 | High slump retaining type polycarboxylic acid water reducing agent with sustained-release effect and preparation method thereof |
| CN103373832A (en) * | 2012-04-17 | 2013-10-30 | 苏琳 | High-performance anti-cracking anticorrosive water reducing agent composition and preparation method thereof |
| CN102911320A (en) * | 2012-07-21 | 2013-02-06 | 北京工业大学 | Method for preparing powder polycarboxylic acid superplasticizer |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749955A (en) * | 2015-11-20 | 2017-05-31 | 衡阳市银利实业有限公司 | A kind of anti-chamotte mould polycarboxylate water-reducer |
| CN106750045A (en) * | 2015-11-20 | 2017-05-31 | 衡阳市银利实业有限公司 | A kind of method for preparing anti-chamotte mould polycarboxylate water-reducer |
| CN106632891A (en) * | 2016-12-27 | 2017-05-10 | 陕西友邦新材料科技有限公司 | Polycarboxylate superplasticizer mother solution based on steam-cured concrete and preparation method of polycarboxylate superplasticizer mother solution |
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