Synthesis and Application of Novel Ecofriendly Powder Detergents of Based on Renewable Raw materials

 

J. R. Dontulwar

Asst. Prof. in Department of Chemistry, Priyadarshini Institute of Engineering and Technology, Hingna Road, CRPF Gate, Nagpur, Maharashtra-440 019, India.

*Corresponding Author E-mail: jdontulwar@yahoo.co.in

 

 

INTRODUCTION:

The specialty of the samples formulated by resin batch 14 is that during formulation of powder detergents the acid slurry percentage has been maintained to minimum level, which runs contrary to the conventional samples of petroleum origin. 

 

In the formulations T₁ to T₅  a systematic study was undertaken to assess the detergent performance by using least quantity of LABS. And in all these formulations polymer percentage has been increased in every formulation and in samples T₃ to T₄ the amount of LABS was reduced to 0.892% and oo% reply. 

 

Altogether the formulations T₁ to T₅ were novel experiment going against the traditional formulations of powder detergents wherein the LABS percentage is to the higher side. The novel ecofriendly polymers can be used as polymeric surfactants which has positive effect on the performance features of detergents viz:

 

1. Calcium magnesium sequisterization

2. Clay soil disperency and soil removal

3. Calcium carbonate inhibition

4. Prevention of soil redeposition

5. Helps to reduce river foaming

6. Prevents Eutrophication

 

In the present research work experimental conditions have been worked out for getting a novel ecofriendly resin based on starch, glycerol sorbitol and maleic anhydride. The procedure has been standardized to get resin of desired molecular weight, HLB ratio.  

 

EXPERIMENTAL:

First Step: - Glycerol, sorbitol, Starch and Maleic Anhydride and little water mixed thoroughly and converted into a homogenous paste by using electrically controlled homogenizer. The paste should have flow and mobility. The paste was introduced into the reactor.

 

Second Step: - The Mass was slowly heated to 80°C in about 15 minutes. The reaction was controlled between +2°C by an accurate heating control.

 

Third Step: - The sample was observed periodically and its consistency was kept free flowing by adding calculated amount of water after every 15 minutes. The samples were checked periodically for Acid value, viscosity and the batch was terminated after 3 to 3½ hr. after getting desired characteristics

 

The six powder detergent formulation prepared as detailed in table. 5. The 92% LABS has been replaced by novel polymer. The % of EDTA has been maintained to constant level 8.92%.

 

A very small proportion of SLS SLES and CMC has been used to have better foaming properties. The table 6,7,8 of surface tension and foam volume describes the effect of detergent concentration on  surface tension  and foam volume  of water. Our samples are on par or sometimes even better than commercial products which were tested simultaneously. The percent detergency was determined using standard soiling techniques on cotton cloth. In this Experiment reflectance of cloth is measured by using digital reflectance meter.

 

RESULTS AND DISCUSSION:

The novel ecofriendly polymers having favorable molecular wt., acid value, HLB has been synthesized using starch glycerol sorbitol andmaleic anhydride. The biodegradation value of polymer was found to be ie BOD to COD ratio is found be 0.5976.    The reaction conditions have been standardized and the reaction is simple but needs constant observation to avoid charring. Hydrochloric acid was used as catalyst to accelerate the rate of esterification. The novel ecofriendly polymer is found to be biodegradable. The novel ecofriendly polymer has been used as 92% replacement of LABS in the formulation of detergent powders. These powder detergents have been analyzed for surface tension, foam volume and percent detergency value as described in table no.6 to 11.

 

Table 01: Synthesis of Polymer Based On Starch, Sorbitol, Glycerol, Maleic Anhydride and

Raw Material	Batch 14(%)
Starch	30.76
Sorbitol	26.92
Glycerol	26.92
Maleic Anhydride	15.38

 

Table 02: Solvent co-solvent catalyst used in the reaction

Solvent co-solvent catalyst	Batch 14(%)
Water	107.69%
Conc. HCl	1.53%

 

Table 03: Cooking Schedule of Polymer 14

Time  in Hrs. min	Temperature (oC)	Remarks
00.00	Room Temperature	600 g water added  and batch started
00.30	48
01.00	75
01.30	95
02.00	100
02.10	101	300 g water added
02.30	103	Thickening of batch started
02.40	105	200 g water added
02.50	106	300 g water added
03.00	108	Batch turned viscous
03.10	108
03.15	116	Batch terminated

 

Table 04: Physico-Chemical Properties Of Polymer  14

Sr. No.	Polymer Property	Observation
1	Acid value of the polymer	57.1
2	pH  value	2.00
3	Saponification value	385.35
4	Solid (%)	64
5	Color	White
6	Solubility of polymer (i) in water (ii) in Xylene (iii) in alcohol + water (iv) in NaOH solution	Soluble In soluble Partially soluble Soluble
7	Hydrophilic Liphophilic Balance of polymer	11.88
8	Molecular Weight of the polymer	1863

 

Table 05: Composition of Powder Detergents of Polymer 14 (Composition % by Weight)

Raw Materials	T1	T2	T3	T4	T5
Polymer (100%)	15.17	16.07	16.96	17.85	8.92
Acid Slurry (100%)	2.67	1.78	0.892	00	8.92
Sodium Carbonate	53.57	53.57	53.57	53.57	53.57
Ethylene DiamineTetraaceticAcid.	8.92	8.92	8.92	8.92	8.92
Sodium tripolyphosphate	4.446	4.446	4.446	4.446	4.446
Sodium Lauryl Sulphate	1.785	1.785	1.785	1.785	1.785
Sodium Lauryl Ether Sulphate.	1.785	1.785	1.785	1.785	1.785
Carboxy Methyl Cellulose.	0.446	0.446	0.446	0.446	0.446
water	12	12	12	12	12

Note: Polymer Was Used As A Solution In Water (74%Solid); Acid Slurry Was Used As A Solution In Water (84%Solid)

 

Table 06: Study of Surface Tension of Water at Various Concentration of Detergent

Sample	Concentration	S.T.in dynes/cm	%Reduction in S.T. of water
T1	0.1	44.86	36.97
	0.25	33.58	55.82
	0.5	25.72	63.86
	1	22.36	68.58
T2	0.1	48.90	31.30
	0.25	41.56	41.61
	0.5	35.62	49.95
	1	31.51	55.73
T3	0.1	54.54	23.37
	0.25	47.04	33.91
	0.5	42.62	40.12
	1	38.43	46.01
T4	0.1	50.68	28.80
	0.25	44.77	37.10
	0.5	40.69	42.83
	1	37.96	46.67
T5	0.1	60.71	14.70
	0.25	55.63	21.84
	0.5	50.47	29.09
	1	40.78	42.70
Surf excel	0.1	46.42	35.61
	0.25	42.66	40.83
	0.5	32.95	54.29
	1	22.85	67.89

Table 07: Study of Foam Volume At 0.1% Concentration of Detergent

Sr.no.	Sample	Foam in Cm3
		Time Volume in Min
		0	5	10	15	20
1	T1	240	210	210	210	210
2	T2	200	200	200	200	200
3	T3	150	150	150	150	150
4	T4	120	120	120	120	120
5	T5	70	70	70	70	70
6	Surf excel	80	80	70	70	70

 

Table 08: Study of Foam Volume At 0.25%Concentration of Detergent

Sr.no.	Sample	Foam In Cm3
		Time volume in Min
		0	5	10	15	20
1	T1	290	270	270	270	270
2	T2	250	240	240	240	240
3	T3	180	180	180	180	180
4	T4	160	160	160	160	160
5	T5	110	110	110	110	110
6	Surf excel	150	150	140	140	140

 

Table 09: Study of Percent Detergency on   Soil Stained Cotton Cloth at Different Concentration of detergent

Ro=Reflectance Measured On Clean Cotton Cloth=80.1

Rs=Reflectance Measured On Soiled Cotton Cloth=22

Rw=Reflectance Measured On Washed Cotton Cloth.

Sr. no.	Sample	Concentration	% Detergency
1	T1	01	73.1
		0.25	73.44
2	T2	0.1	72.58
		0.25	76.54
3	T3	0.1	71.20
		0.25	75.33
4	T4	0.1	69.83
		0.25	71.89
5	T5	0.1	69.66
		0.25	72.41
5	Surf excel	0.1	76.49
		0.25	80.26

Table 10:  Study of Percent Detergency on Tea Stained Cotton Cloth at Different Concentration of detergent

Ro=Reflectance Measured On Clean Cotton Cloth=80.1

Rs=Reflectance Measured On Tea cotton Cloth=33

Rw=Reflectance Measured On Washed Cotton Cloth

Sr.no.	Sample	Concentration	% Detergency
1	T1	01	77.95
		0.25	80.54
2	T2	0.1	75.70
		0.25	77.97
3	T3	0.1	68.36
		0.25	73.03
4	T4	0.1	66.44
		0.25	72.07
5	T5	0.1	64.51
		0.25	69.67
5	Surf excel	0.1	76.49
		0.25	80.26

 

Table 11: Study of Percent Detergency on   Coffee Stained Cotton Cloth at Different Concentration of detergent

Ro=Reflectance Measured On Clean Cotton Cloth=80.1

Rs=Reflectance Measured On Coffee Cotton Cloth=29

Rw=Reflectance Measured On Washed Cotton

Sr.no.	Sample	Concentration	% Detergency
1	T1	01	81.37
		0.25	86.26
2	T2	0.1	78.85
		0.25	83.03
3	T3	0.1	76.49
		0.25	81.68
4	T4	0.1	74.84
		0.25	79.73
5	T5	0.1	73.96
		0.25	77.45
5	Surf excel	0.1	76.49
		0.25	80.26

 

The various green compositions are good to excellent in comparison to commercial samples of petroleum origin in which conventionally up to 45% to 50% of LABS, 35 %to 40%  of STPP is used.

 

While studying the surface tension of water at various concentration of detergent it was found that keeping LABS level to bare minimum i.e. 0.89% ando.oo% in formulations like T3, T4 the ability of detergent to minimize the surface tension of water was found to be excellent as compare to the commercial sample ex. Surf excel.

 

It is evident from table 6, which explains the impact of detergent on surface tension of water at various concentrations. The sample T₃ andT₄ reduces the surface tension of water  0.1 gm of detergent/ 100gm of water by 23.37% and 28.80 respectively. Whereas commercial sample surf excel can reduce the  surface tension of water at 0.1 gm of detergent/ 100gm of water by 35.61%.

 

This difference in the values of surface tension between surf excel and T₃ and T₄ sample must be because of bare minimum percentage of LABS in sample T₃and T₄ which is happens to be principal component of commercial sample i.e. surf excel.Inspite of less percentage of LABS the powder detergents perform well. This leaves scope for the promotion of pure polymeric detergent keeping LABS percentage sometimes to zero level.

 

The study of surface tension of water at 0.25 gm of detergent/100gm of water exhibit  the similar trend to that of 0.1 gm /100 gm of water.

 

The study of foam volume at various concentration of detergent for instance at 0.1 gm of detergent/ 100gm of water and 0.25 gm of detergent/100gm of water ref.table 7,8 the samples from T1 to T5  shows excellent performance as compared to commercial sample.

 

Finally the very important study which shows the actual and practical performance of detergent ie.the study of percent detergency was conducted on various stained cotton cloth ie. Soil, Tea, Cotton etc.

 

This study helps to know the cleaning action of detergents. The percent detergency value of powder detergents starting from T1 to T5 was found to be appreciable although slightly lesser than commercial sample as seen from table 9.This slightest difference in the cleaning action of commercial sample ie.surf excel may be because of petroleum products.

 

Similar expt. was carried on Tea stained cotton cloth. As seen from table 10 the cleaning action of T1 was even better than commercial one but T₂ to T₅ have less cleaning action owing to lesser percentage of LABS than surf excel.

 

The combined study of surface tension, foam volume, percent detergency of powder detergents of polymeric origin reveals that a kind of paradigmatic shift in the formulation of detergents is absolutely possible without compromising the performance potential of detergents.

 

The samples T₁ to T₅ containg least percentage of petroleum origin products like STPP (4.446%), SLS (1.785), SLES (1.785), CMC (0.446%) can be formulated and these samples perform well. These formulations pave the way for pure, renewable, biodegradable polymeric detergents and its marketization for the masses at reasonable cost. Such kind of experiments will encourage the diversification of agriculture towards value added products by sustainable approach.

    

REFERENCES:

1.       Zini, Paolo Polymeric Additives High Performance Detergence (Technomic Publishing Company INC Lancaster BASEL,1995 p 15,42)

2.       Gogte B.B., Agrawal R. S., Pandharipande S. L., Detergent Formulation by ANN (Chemical Engineering World Vol 38, No. 5, p 78,8, 2003)

3.       Gogte B.B., Agrawal R. S., Pandharipande S. L., Badhe Y.P. Starch Sorbitol based co-polymer ,  A substitute for LABS (Soaps,Detergent and Toiletries review p 24,28, April 2003)

4.       K.S.Parsuram,”Soaps and Detergents “, Tata Mc Graw –Hill p.p162, 164 165, 172, 173,175, 1995.

 

ABBREVIATIONS:

LABS: Linear Alkyl Benzene Sulfonate

HLB: Hydrophilic Liphophilic Balance

SLS:Sodium Lauryl Sulphate

SLES: Sodium Lauryl Ether Sulphate

CMC: Carboxy Methyl Cellulose

BOD: Biological Oxygen Demand

STPP: Sodium Tri poly phosphate

 

 

 

Received on 12.06.2013       Modified on 22.06.2013

Accepted on 25.06.2013      © AJRC All right reserved