Synthesis of Polycarboxilate

International Conference on Materials, Environmental and Biological Engineering (MEBE 2015)
Synthesis on a type of polycarboxylate superplasticizer under room

temprature
Xing Li1,a , Minghua Yuan1, Chong sun1 , Jinwen Wang1
1
China Construction Ready Mixed Concrete Co. Ltd, Wuhan 430205, China,
a
leexingbridge@yeah.net,
Keywords: polycarboxylate superplasticizer, temprature, fluidity of cement paste, concrete slump
Abstract. This investigation was undertaken to evaluate a new kind of polycarboxylate

superplasticizer .Used polyoxyethylene ether (TPEG), acrylic acid (AA) functional monomer
(A)and as the monomer, hydrogen peroxide (H2O2) as initiator, Vitamin C (Vc)as reducing agent,
TGA as chain transfer agent, synthesised polycarboxylate superplasticizer with high water reducing
rate under 15 C ~ 27 C. The effect of admixtures on fluidity and concrete slump were discussed in
this paper..This investigation also evaluated the influence of different serials of polyoxyethylene
ether, the dosage of hydrogen peroxide (H 2 O 2 ) and Vitamin C (Vc).
1 Introduction
Concrete is the world's the largest building materials, widely used in various construction
projects. Chemical admixture plays an important role in concrete, it could reduce water
consumption and dispersion of cement particles, increase the strength of concrete, etc[1].
Polycarboxylate superplasticizers are the most important water reducing agent[2-4]. It replaced
first generation and second generation water reducing agent, such as lignin sulfonate, naphthalene
water reducer and aliphat sulfate water reducer. It solved fast slump loss of naphthalene water
reducer and delayed coagulation of lignin sulfonate[5]. In terms of chemical structure,these
polymers have lots of advantages: better fluidity and slump flow with low dosage of PCs, wide
adaptability for cement,higher water-reducing efficiency,large freedom of molecular structure,more
synthesis technology,more room for improvement[6-7].
Most polycarboxylate superplasticizers adopt radical polymerization under 60-80C, use persulfate
as initiator[8-9]. Quantity of heat was needed during its synthesis. This could bring environment
pollution, consume lots of energy[10]. Sythsis under room tempreture mean a lot to save energy and
reduce the pollution of the environment.
2 Experimental
2.1 Chemicals and Equipment.
Prenyl alcohol ethoxylates (TPEG, Liaoning Kelong Chemical Co. LTD), Acrylic acid
(AA,Wuhan Zhonghua Yongye Chemical Co. LTD),
Hydrogen peroxide (H2O2, Wuhan
chemical Co. LTD), Vitamin C (Vc, Wuhan zhongxin materials Co.LTD), Chain transfer agent
(TGA, Changzhou Yurong Chemical Co.LTD) ,sodium hydroxide(NaOH), HuaXin
cement,P.O42.5,WuGang II flyash, WuXin S95 silica fume. Cement paste mixer,NJ-160A,WuXi
JianYi equipment Co. LTD ; Single horizontal-axis laboratory concrete mixer,HJW-60,ShenYang
JuLin equipment Co. LTD.
2.2 Synthesis Process.
Put water and TPEG into a flask, and stirried until the end of experiment; wait until TPEG
dissolved, then added the H 2 O 2 at 60oC, and dripped the AA , functional monomer (A), Vitamin C
(Vc)and TGA solution; keep stirring for certain hours, then added the sodium hydroxide and water,
and adjusted pH of the new product about 7; The new product would been gotten and its solid
content was 40%.
2015. The authors - Published by Atlantis Press
209
2.3 Measurement.
The fluidity of cement slurry was tested according
(GB/8077-2000).The water-cement ratio is 0.29,PCs dosage is 0.13%.
to
Chinese
Standard
3 Results and Discussion

3.1 Determination of monomer type
F108 and TJ-188 are synthesised by imported initiator, while F1088 and TJ-188C are
synthesised by domestic initiator. The front two kinds of monomers are more active than back ones.
The table shows F108 and TJ188 is more suitable for this method.
Table.1 Fluidity of cement paste with different monomer condition of PCs
Type
F108(Liaoning Kelong Chemical Co.
LTD )
F1088(Liaoning Kelong Chemical Co.
LTD )
TJ188(ShangHai TaiJie Chemical Co.
LTD )
TJ188C(ShangHai TaiJie Chemical Co.
LTD )
0min Slump flow(mm)

240/565
60min Slump flow(mm)

230/560
240/560
220/480
250/590
230/580
235/540
225/470
Fluidity of cement paste
3.2 Determination of initiator Dosage

We can see from figure 1, with all other conditions being equal, concrete has the best dispertion
performance when the dosage of initiator is 0.015mol. This is because low dosage of initiator
causes little active centre, reaction is not complete; as high dosage of initiator causes too many
active centre, the molecular weight is too small to the disadvantage of space steric hindrance.
350
300
250
200
F108
TJ188
150
100
50
0
0
0.005
0.01
0.015
0.02
Initiator dosage
0.025
0.03
Fig.1 Fluidity of cement paste with different density of initiator

3.3 Determination of reaction time
According to time temperature equivalence principle, we studied the influence of reaction time
on the properties of polycarboxylate superplasticizers. We can see from figure 2 that 4h is the most
suitable reaction time: reaction is not complete less than 4h, it is helpless more than 4h.
210
Fluidity of cement paste
350
300
250
200
F108
TJ188
150
100
50
0
0
4
Reaction time
Fig.2 Fluidity of cement paste with different reaction time

4 Conclusion
By discussing various factors that impact the performance of PCs, we confirm a suitable
process conditions which a
new
type
of
polycarboxylate
superplasticizer
was
synthesized under room tempreture. The influencing factors of reaction include proportion
of initiator concentration and reaction time. It is possible to realize industrial production under
room tempreture, then save energy and reduce the pollution of the environment.
References
[1] J. Witt, J. Plank, A Novel type of PCE possessing Silyl Functionalities, In print.
[2] Liping G, Shaofeng W, Anfu Z, et al. Determination of Residual Monomers in Polycarboxylate
Superplasticizer Using High Performance Liquid Chromatography[J]. Journal of Wuhan University
of Technology(Materials Science Edition), 2011, (3): 439-442.
[3] Yamada K, Takahashi T, Hanehara S, et al. Effects of the Chemical Structure on the Properties
of Polycarboxylate-type Superplasticizer[J]. Cement and Concrete Research, 2000, 30(2): 197-207.
[4] K.Yamada,S.Ogawa, S, Hanebara, Controlling of the Adsorption and Dispersing Force of
Polycarboxylate type Superplasticizer by Sulfate ion Concentration in Aqueous Phase, Cem. Concr.
Res.31(2001) 375-383.
[5] Plank J, Brandl A, Zhai Y, et al. Adsorption Behavior and Effectiveness of
Poly(N,N-dimethylacrylamide-co-Ca 2-acrylamido-2-methylpropanesulfonate) as Cement Fluid
Loss Additive in the Presence of Acetone-formaldehyde-sulfite Dispersant[J]. Journal of Applied
Polymer Science, 2006, 102(5): 4341-4347.
[6] Guo M, Que C, Wang C, et al. Multifunctional Superparamagnetic Nanocarriers with
Folate-mediated and pH-responsive Targeting Properties for Anticancer Drug Delivery[J].
Biomaterials, 2011, 32(1): 185-194.
[7] Lowke D, Krnkel T, Gehlen C, et al. Effect of Cement on Superplasticizer Adsorption, Yield
Stress, Thixotropy and Segregation ResistanceDesign, Production and Placement of
Self-Consolidating Concrete[J]. 2010, 1: 91-101.
[8] C. Li, H. Wang, H. Wu, et al, Synthesis and performance a slowly-released type polycarboxylic
water-reducers, Baton Chinese Edition-ready-mixed Concrete, 10 (2010) 27-28.
211
[9] Z. Wang, Polycarboxylate Superplasticizer--Preparation Performance and Application, China

Building Industry Press, Beijing, (2009) 153-201.
[10] S. Li, Q. Yu, J. Wei, Effect of molecular structure of polycarboxylate water
reducers on
hydration of cement, Journal of the Chinese Ceramic Society, 4 (2012) 614-618.
212

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International Conference on Materials, Environmental and Biological Engineering (MEBE 2015)

Synthesis on a type of polycarboxylate superplasticizer under room

Keywords: polycarboxylate superplasticizer, temprature, fluidity of cement paste, concrete slump

Abstract. This investigation was undertaken to evaluate a new kind of polycarboxylate

2015. The authors - Published by Atlantis Press

3 Results and Discussion

0min Slump flow(mm)

60min Slump flow(mm)

Fluidity of cement paste

3.2 Determination of initiator Dosage

Fig.1 Fluidity of cement paste with different density of initiator

Fluidity of cement paste

Fig.2 Fluidity of cement paste with different reaction time

[9] Z. Wang, Polycarboxylate Superplasticizer--Preparation Performance and Application, China

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