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

 

J.R. Dontulwar

Priyadarshini Institute of Engineering and Technology, Nagpur-440019, India

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

 

 

ABSTRACT:

Various liquid detergents were formulated using ecofriendly polymer of mixed carbohydrate and glycol and anhydride origin. The samples were showing excellent results in terms of performance like reduction in surface tension of water, foam volume and percent detergency. The samples have shown good performance at par with conventional samples of petroleum origin.

 

KEYWORDS: Ecofriendly polymer, foam volume, percent detergency

 

 

INTRODUCTION:

In the present context there is global trend towards use of liquid detergents because of their convenience, ease of dispensation and dispersion in water, owing to such characteristics liquid detergents are gaining popularity. From manufacturing angle liquid detergents can be manufactured using relatively simple equipments. Liquid detergents are of various types

 

1. Heavy duty liquid detergents for regular washings

2. Light duty liquid detergents wool, silk etc.

3. Dish washing liquid detergents.

 

In the present work few green liquid detergents were formulated using diethanol amine neutralized polymer and acid slurry.  Liquid detergents formulated using diethanol amine neutralized  carbohydrate polymers and slurry have shown good results in terms of performance like reduction in surface tension of water, foam volume, percent detergency. Neutralization using diethanol amine neutralization has brought excellent appearance, feel and color to the samples of liquid detergents. In the previous work1 the synthesis and characterization of biodegradable polymers from starch, glycerol, sorbitol and maleic anhydride was discussed. The synthesis and application of detergent from above source was also discussed2.  

 

The resin manufactured from starch, sorbitol, glycerol, maleic anhydride is found to be biodegradable in nature3. The various powder detergents were formulated using starch, , glycerol ,maleic anhydride resin4 and used in cleaning of cloth successfully and various liquid detergents were formulated using different resin.5,6

 

EXPERIMENTAL:

Table-1 describes the composition of the green polymer.

Raw Material

Batch 14(%)

Starch

30.76

Sorbitol

26.92

Glycerol

26.92

Maleic Anhydride

15.38

Phthalic Anhydride

Nil

 

Table 2 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 3 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

BOD TO COD Ratio

0.5967

9

Molecular Weight of the polymer

1863

 

Preparation of Liquid Detergent

Various Raw Materials in liquid detergent like Neutralized Acid Slurry neutralized polymeric resin and conventional ingredients were taken in a glass reactor and homogenized by running the stirrer for about half an hour. Refer. Table 1.2.2

 

The Solution is cooled in refrigerator at 10°C for 48 hrs. The clear liquid solution was filtered and packed in superior grade air tight plastic containers.

 

 

Table 4 Composition of Liquid Detergent Using Di-Ethanol Amine Neutralized Polymer-14 (By % Weight Method)    

Raw Materials

F1

F2

F3

F4

Neutralized acid slurry (100%)

5

5

5

5

Neutralized polymer (100%)

5

5

5

5

Sodium Lauryl Sulphate

2

2

2

2

Sodium Lauryl Ether Sulphate

2

2

2

2

Carboxy methyl cellulose

1

1

1

1

Ethylene Diamine Tetra-  Acetic Acid

5

3

2

1

Sodium Sulphate

5

7

8

9

Urea

5

5

5

5

Water

70

70

70

70

Note Di-ethanol amine neutralized polymer was used as a solution (22%solid)

Di-ethanol amine neutralized acid slurry was used as a solution (13%solid)

 

Study of surface tension of water

The Stalagnometer Method   

The stalognometer consist of a pipette like tube having smooth capillary end with sharp edges. It is filled with the liquid up to the mark by sucking at the upper end of the tube. The liquid is their allowed to come down in the form of drop. Each drop coming out of the capillary end goes all increasing in size to a certain point and then falls down. The ultimate size of the drop depends upon the radius of the capillary orifice and the surface tension of the liquid.

 

The drop is supported by the source of surface tension, 2p rn where r is the radius of the drop at the end of the capillary tube. The drop falls when its weight W just exceeds the force of surface tension A moment before, at equilibrium.

 

W = mg = 2p r n

Where, m is the mass of the drop and g is the acceleration due to gravity. Knowing the surface tension of the one liquid. We can calculate the surface tension of the other liquid easily by using following formula.

 

                             

Where,

g1 = Surface tension of the sample

g2 = Surface tension of water i.e. 71.8 dynes/cm.

P1 = Density of sample

P2 = Density of water (0.997gm/cm3)

n1 = No. of drops of sample

n2 = No. of drops of water

 

These are four methods used for determining the surface tension of the samples among which we have used stalgnometer method.

 

 

Table 5 Study of Surface Tension of Water at Various Concentration of Detergent

Sample

Concentration

(%)

Surface Tension (Dynes/Cm)

% Reduction In Surface Tension  of Water

 

F1

0.1

46.07

35.27

0.25

40..65

42.89

 

F2

0.1

43.37

39.06

0.25

37.86

46.81

 

F3

0.1

39.77

44.12

0.25

35.53

50.08

 

F4

0.1

36.17

49.18

0.25

31.08

56.33

Surf excel liquid

0.1

16.28

77.13

0.25

15.95

77.59

 

Foam Volume3 Foam volume was determined by using bubble cylinder method

1) Bubble Cylinder Method: Foam characteristics are measured in terms of volume and the following steps are carried out for it.

 

Take 1000 ml cylinder provided with stopper, add to it 100 ml solution of particular concentration whose foam characteristics is to be measured. Give it 30 up-down rotation within time period of 30 seconds. Keep that cylinder on table and observe the foam above liquid level and note down reading at min. The readings were measured after 5, 10, 15 min. respectively. Same procedure is carried out for the solution at different concentration like 0.1%, 0.25%, 0.5% and 1.0%

 

 

Table 6 Study of Foam Volume At 0.1 % Concentration of Detergent

Sr.No.

Samples

Foam Vol. In Cm3

0

5

10

15

20

1

F1

200

200

200

200

200

2

F2

230

220

220

220

220

3

F3

160

160

160

160

160

4

F4

210

210

210

210

210

5

Surf excel liquid

121

119

111

111

111

 

Table 7 Study of Foam Volume At 0.25%Concentration of Detergent

Sr. No.

Samples

Foam Vol. In Cm3

0

5

10

15

20

1

F1

400

400

400

400

400

2

F2

450

450

450

450

450

3

F3

380

380

380

380

380

4

F4

360

360

360

360

360

5

Surf excel liquid

142

133

131

118

118

 

 

Percent detergency

a) Soil medium: The soil medium was prepared by mixing Carbon (28.4 %), coconut oil (35.8 %), lauric acid (17.9 %) and mineral oil (17.9 %).

 

b) Preparation of soil solution: This was prepared by adding2 g of above soil paste in 500 ml of carbon tetrachloride solution. Mix it well and use for further cloth sample preparation.

The solution was filled in packed bottle.

 

c) Method of application: The cotton cloths of size 24 cm ×32 cm were prepared. Take 50 ml of soil solution in beaker. Dip this cloth sample in it for 5 min. The same cloth dried in open atmosphere for 2 h. Then this cloth was cut into test sample size of 6 cm × 8 cm and these samples were used for washing purpose. The solutions of different concentration of detergent were prepared and heated to 60 °C temperature. Soiled cloth sample was dipped in it for 5 min and given to and fro 10 hand washes. Washing was carried out in distilled water only. After rinsing these samples in fresh water are kept for drying purpose. The samples which were washed, dried and ironed were used to find out per cent detergency.  The %detergency was determined using lamberts and sanders formula.

Percent detergency

 

Where, Rw, Rs and Ro are reflectance measured on washed cloth, soiled cloth and clean cloth, respectively. The reflectance of the cloth samples were measured by using reflectance meter manufactured by Universal Engineering, Corporation, Ambala Road, Saharanpur. This was standardized by using the magnesium oxide or tile which was provided along with the instrument. This tile having brightness of 81.3 %was adjusted using the knob provided on instrument. After adjustment was done the samples were kept on the instrument

 

And the readings were noted down and the percent detergency was calculated (Table-1.4.1).

 

1 Method of Application (Tea and Coffee)

The cotton cloth of size 24 x 32 cm2 were taken and make checks with the help of size 6 x 8 cm2. Then take the above staining solution in a pipette and add in a center or checks one drop and then kept the stain cloth sample in oven at 100-105°C for half an hour. Then this stained cloth is cut into test sample size and these samples were used for washing purpose

 

Table 8 Study of Percent Detergency at Various Concentration of Detergent on Soiled Stained Cotton Cloth.

Sr. No.

Sample

Concentration

% Detergency

1

F1

0.25

66.56

 

0.5

77.88

2

F2

0.25

62.78

 

0.5

67.76

3

F3

0.25

62.09

 

0.5

65.53

4

F4

0.25

60.71

 

0.5

64.15

5

Surf excel liquid

0.25

75.32

 

0.5

78.62

Ro=Reflectance measured on clean cotton cloth=80.1

Rs= reflectance measured on soiled cotton cloth=40.1

Rw=reflectance measured on washed cotton cloth

 

Table 9 Study of Percent Detergency at Various Concentration of Detergent on Tea Stained Cotton Cloth.

Sr. No.

Sample

Concentration

% Detergency

1

F1

0.25

76.68

 

 

0.5

84.67

2

F2

0.25

74.30

 

 

0.5

83.16

3

F3

0.25

69.76

 

 

0.5

80.35

4

F4

0.25

65.44

 

F1

0.5

76.89

5

Surf excel liquid

0.25

76.30

 

 

0.5

77.20

Ro=Reflectance measured on clean cotton cloth=80.1

Rs= reflectance measured on tea cotton cloth=41.5

Rw=Reflectance measured on washed cotton cloth

Table 10 Study of Percent Detergency at Various Concentration of Detergent on Coffee Stained Cotton Cloth

Sr. No.

Sample

Concentration

% Detergency

1

F1

0.25

80.34

 

 

0.5

84.43

2

F2

0.25

79.36

 

 

0.5

82.68

3

F3

0.25

74.68

 

 

0.5

78.97

4

F4

0.25

70.98

 

 

0.5

77.22

5

Surf excel liquid

0.25

72.24

 

 

0.5

75.10

Ro=Reflectance measured on clean cotton cloth=80.1

Rs= reflectance measured on tea cotton cloth=44.8

Rw=Reflectance measured on washed cotton cloth

 

RESULTS AND DISCUSSION:

As evident from Table-1. that a green carbohydrate polymer was synthesized using 30.76% Starch, 26.92% sorbitol, 26.92% glycerol and 15.38% maleic anhydride having BOD to COD ratio 0.5976 showing biodegradability. The carbohydrate polymer having good molecular wt. and has shown HLB ratio 11.88 suggesting its application in detergent formulation.

 

Various liquid detergents were formulated by varying percentage of various constituents to observe the possible difference in performance characteristics of liquid detergents at changed composition of active components of detergents. The formulations F1 to F4 have different proportion of active components of detergency. (Refer Table4). In all those formulation the complexing agent EDTA varied from five to one percent is usually incorporated in premium quality detergents owing to its cost. Percentage of usually incorporated cheap sodium sulfate was varied from 5 to 9. In all the formulation the polymer and slurry percentage equally maintained. As evident from Table 4 that all detergents have shown pH value 8 and in alkaline medium better detergency is obtained. All samples have shown reasonably good viscosity and density. Every detergents performance is evaluated on the basis of its effects on various functional parameters like effect of detergents on surface tension of water, foam volume of water and percent detergency of cloth.

 

As seen from Table.5 that the samples F3 and F4 have shown good performance in terms of reduction of water  at 0.1and 0.25 percent concentration of detergent which helps in the wetting of cloth in minimum of water but performance is lesser than commercial samples.

 

As evident from tables 6, 7 that F series detergents containing diethanol amine neutralized polymer and acid slurry have shown excellent performance in terms of foam volume. The samples F2 and F4 have shown remarkably good foam stability at lower concentration of detergents.

 

The functionally more important property of detergent is percent detergency. As seen from Table 8 that the sample F1 and F2 have shown 66.56%,77.88%,62.78%,67.76% percent detergency on soiled stained cotton cloth at o.1% and 0.25% concentration of detergents. The similar kind of performance is seen on tea stained and coffee stained cloth as evident from Table 9 and 10.

 

CONCLUSION:

The detergent formulation using ecofriendly polymers and acid slurry are giving excellent performance and sometimes better than commercial petroleum based detergents. The combined study of surface tension, foam volume, percent detergency indicates that foam rich diethanol amine neutralized polymer and acid slurry  exhibit excellent performance and sometimes better than commercial samples. Such kind of detergent formulations can be promoted as ecofriendly foam rich detergents with rich feel, look and performance.

 

ACKNOWLEDGEMENT:

Author is thankful to D. K. Borikar and S.R. Kargirwar for their valuable work.

 

REFERENCES:

1.       Biodegradation and spectroscopic study of polymer synthesized from starch, glycerol, sorbitol, maleic anhydride as precursor. J.R. Dontulwar, D.K. Borikar Asian Journal of Research in Chemistry , July 2011,Volume 4(7) pp 1084-1086.

2.       Synthesis and application of Green Liquid Detergents based on diethanolamine neutralized polymer and acid slurry. J.R. Dontulwar, Asian Journal of Research in Chemistry , 2012 Sept, Volume 23(6) pp 1186-1189.

3.       Biodegradation studies of selected polymers of carbohydrate origin. J.R. Dontulwar, D.K. Borikar.  Asian Journal of Research in Chemistry, 2011 July, 5 (2), pp 197-199.

4.       Synthesis of ecofriendly powder detergents based on starch, glycerol and maleic anhydride. J.R. Dontulwar, Soaps, Detergents and Toiletries Review, 2009 April pp 12-16. 

5.       Synthesis of Eco-friendly detergents by using white dextrin, Sorbitol, Maleic anhydride. J.R. Dontulwar, B.B. Gogte , Asian Journal of Chemistry, 2004, 16, pp 1385-1390.

6.       Synthesis of Green Liquid Detergents using Carbohydrate Polymers Based on White Dextrin, Sorbitol and Maleic Anhydride. J.R. Dontulwar, D.K. Borikar, Asian Journal of    Chemistry, 2011, Volume 236, pp 2511-2514.

 

 

 

 

Received on 21.05.2013       Modified on 26.04.2013

Accepted on 31.05.2013      © AJRC All right reserved

Asian J. Research Chem. 6(5):  May 2013; Page 474-477