Title of Invention

"A FLUID LOSS CONTROL AGENT"

Abstract A process for the preparation of fluid loss control agent for use in the oil well drilling and textile printing comprising in the steps of stirring tamarind kernel powder (TKP) with aqueous methanol containing sodium hydroxide and refluxed on a water bath, cooling the reaction product and adding monochloro acetic acid with continuous stirring and than refluxing the same on a water bath cooling said mixture and adding sodium hydroxide thereto, refluxing the product and cooling the same, filtering and washing till the filtrate has a PH 9 to 11.
Full Text FIELD OF INVENTION
This invention relates to a process for the preparation of methyl tamarind kernel powder (TKP) for use as a fluid loss control agent oil well drilling and in the textile printing.
PRIOR ART
Various fluid loss additives like starch, pregelatinised starch, CMC, PAC (Polyanionic Cellulose) etc. are known and the use of fluid loss additive is well established to be added with various kind of drilling fluids to control filtration characteristics. The requirements to use the fluid loss additives are i) no increase in viscosity ii) compatibility with mud system iii) resistance to temperature deterioration iv) reduction of fluid loss to the desired level by the addition of small quantity in order to minimize expenditure.
There are certain disadvantages associated with the use of the conventional fluid loss control agents. One of the main disadvantage is that the use of the conventional agents is very costly.
Another disadvantage is that the conventional agents are not so efficient as in the oil well drill industries.
OBJECT OF THE INVENTION
A primary main object of this invention is to propose a novel fluiti loss control agent which fulfills the above mentioned requirement for use in the oil well industries and textile industries.
According to this invention there is provided a process for she preparation of a fluid loss control agent for use in the oil weli drilling und textile printing comprising in the steps of stirring tamarind kernel powder (TKP) with aqueous methanol containing sodium hydroxide and refluxed on a water bath, cooling the reaction product and aiding rnonochloro acetic acid with continuous stirring and than rei'Suvm;., ih<. same on a water bath cooling said mixture and adding sodium hydroxide thereto refluxing the product filtering arid washing till filtrate has ph to> In accordance with this invention fluid loss additives are added to various types of drilling fluids for control of filtration characteristics. They interact with clay to yield a thin dense impermeable cake at the wall of the bore hole. According to the type, they can also make an important contribution in controlling the rheology of the mud. The basic requirement of fluid loss additives are:
1. No viscosity increase
2. Compatibility with mud system
3. Resistance to temperature deterioration
4. Reduction of fluid loss to the desired level by addition of small
quantities thereby incurring less expenditure.
TKP was stirred with aq. Methanol (H2O: Methanol : : 5 : 95 to 95 : 5) in 1 : 2 ratio containing sodium hydroxide 5 to 50% of the weight of TKP in round bottom flask. The material was stirred for 5-60 mts and refluxed on a water bath for 1 to 6 hrs.
Product was cooled to room temperature and monochloro acetic acid 5 to 50% of the weight of TKP was added with

continuous stirring and temperature maintained at 30-40" C. It was refluxed on water bath for 1-4 hr. and cooled to room temperature, filtered and washed with aq. methanol until the pH of the filtrate is 9 to 11^. Product was dried and pulverised to 100-200 mesh. Degree of substitution of the product 0.01 to 1 was obtained and used as additive in fluid loss control.
Further objects and advantages of this invention will be apparent from the ensuing example.
EXAMPLE
TKP (100 g) was stirred in aq. methanol (200 ml, methanol -water ::80:20) containing sodium hydroxide (25-50 g) and refluxed on a water bath for 1 hr. Product was cooled to room temperature and monochloro acetic acid (25-50 g) in HZO-CH3OH (20:80, 100 ml) was added slowly with stirring. It was refluxed on a boiling water bath for 3 hr. The product was cooled at room temperature, was filtered under vacuum and washed twice with aq. methanol (~ 2 x 50 ml). Product was spread initially on a polythene sheet for air-drying at room temperature (10 -30 mts) and finally dried in hot

air oven at 70 - 80°C (1 hr.). Product so obtained was pulverised (100 mesh) having DS 0.02-0.40, protein (2.50-1.258), pH (11.22%, 1% solution).
Rheological studies of the product was carried out using Brookfield viscometer. Viscosity of the 4% solution (table - 1) shows non-newtonian nature of the product.
Table - 1 Viscosity of 4% solution of TKPM (DS 0.334) at 25° C, spindle 27

(Table Removed)
Results indicate viscosity of the product remains stable upto 72 hr and as a matter of fact increases upto 1.25 times.
Viscosity of 4% solution of TKPM in 5% Sodium chloride is given in table -- 2. It shows increase in the stability and viscosity in saline water.
Table-2 Viscosity of 4% solution of TKPM (DS 0.334) in 5% NaCl, at 25° C, spindle 27

(Table Removed)
Viscosity of TKPM remains stable in saline water upto 72 hr which is normally not the case with galactomannan. Increase in viscosity in saline water after 72 hr is 1.4 times in comparison to initial viscosity taken after 3 hr.
Viscosity vs temperature of TKPM was measured by programming the viscometer (temperature increase 5" C/min., hold time 1 min., chart speed 20 cm/hr). Data is shown in table-3.
Table - 3 Viscosity vs Temperature of 4% TKPM (I)S 0.334). spindle 27
(Table Removed)
Table shows decrease in viscosity as the temperature increases. Viscosity decreases drastically from 4175 Cps at 25°C to 525 Cps at 95°C.
Synergism with xanthan gum
Synergistic studies of TKPM with xanthan gum was carried out. TKPM (2g) in 65 ml water (3.07%) was taken as control and 0.1 g and 0.05 g xanthan dissolved separately in 15 ml water was added to TKPM solution (2 g in 50 ml) respectively. In other words, xanthan solution and TKPM solution when added together and stirred for synergistic action is having TKPM : Xanthan :: 1 : 20 and 1 . 40 ratio (w/w).
Procedure adopted for synergism is as follows:
TKPM (4%, 2g in 50 ml) solution was prepared at 55-60 ° C with stirring for one hour and allowed to cool at ambient temperature.
Xanthan (100 mg or 50 mg) was dissolved in 15 ml water at 60-70° C with stirring for 10 minutes and allowed to cool at ambient temperature.
TKPM and Xanthan solutions were mixed together with stirring for 10 - 15 minutes and viscosity was measured. Increase in viscosity of TKPM in distilled water and saline water due to synergistic action of xanthan is shown in table - 4.
Table-4 Synergistic action of xanthan gum with TKPM (DS 0.334) in distilled water, temperature 25 ° C, spindle 27.

(Table Removed)
Table-2 a"hd Table-4 shows the viscosity of TKPM increases in saline water, with or without xanthan gum. Viscosity of the TKPM in fresh water and saline water also remains stable or increases in fresh/saline water upto 72 hr without any addition of biocide or preservative.
TKPM (DS 0.334) serves to decrease fluid loss, a measure of the tendency of the liquid phase of the drilling fluid to pass through the filtrate cake into the formation.
Test report of the Product as fluid loss control agent is as follows:
(Table Removed)
8. Performance test in salt water mud
(a) Base mud: Added 4% NaCl to
10% bent.Susp. hydrated at 90 ± 2" C
for 72 hrs. and aged for 24 hrs.
24 ± 2° C temp. (pH 9.0-9.5).
Diluted with 4 % salt water to get
(i) Apparent Viscosity Cp 155
(ii) Yield Point Lbs/100 sq.ft. 23.0
(iii) API water loss ml. 52.0
(b) Treated the base mud 8(a) with
0.5% (w/v) TKPM sample, stirred for
15 min. at high speed in Hamilton
Beach Mixer
(c) Performance at 24 + 2 ° C:
Determined following parameters
of mud as per 8 (b)
(i) Apparent Viscosity Cp 8.0
(ii) Yield Point Lbs/100 sq. ft. 4.0
(iii) API water loss ml. 47.0



WE CLAIM:
1. A process for the preparation of a fluid loss control agent for use in
the oil well drilling and textile printing comprising in the steps of
stirring tamarind kernel powder (TKP) with aqueous methanol
containing sodium hydroxide and refluxed on a water bath, cooling
the reaction product and adding monochloro acetic acid with
continuous stirring and than refluxing the same on a water bath
cooling said mixture and adding sodium hydroxide thereto, refluxing
the product and cooling the same, filtering and washing till the filtrate
has a pH 9 to 11.
2. A process as claimed in claim 1 wherein the aqueous methanol has a
water to methanol ratio of 5 : 95 to 95 : 5.
3. A process as claimed in claim 1 wherein said aqueous methanol and
TKP contains 5 to 50% by weight of TKP.
4. A process as claimed in claim 1 wherein the mixture is refluxed in a
water bath for 1 to 6 hours to obtain a reaction product.
5. A process as claimed in claim 5 wherein 5 to 50% by weight
monochloro acetic acid is added to the reaction product under stirring
at a temperature of 30 to 40° C.
6. A process for the preparation of a fluid control agent substantially as herein described and illustrated in the example.


Documents:

681-del-2000-abstract.pdf

681-del-2000-claims.pdf

681-DEL-2000-Correspondence-Others-(26-06-2008).pdf

681-del-2000-correspondence-others.pdf

681-del-2000-correspondence-po.pdf

681-del-2000-description (complete).pdf

681-del-2000-form-1.pdf

681-DEL-2000-Form-15-(26-06-2008).pdf

681-del-2000-form-19.pdf

681-del-2000-form-2.pdf

681-DEL-2000-Form-26-(26-06-2008).pdf

681-del-2000-form-26.pdf

681-del-2000-form-5.pdf

681-del-2000-petition-others.pdf


Patent Number 209450
Indian Patent Application Number 681/DEL/2000
PG Journal Number 40/2007
Publication Date 05-Oct-2007
Grant Date 30-Aug-2007
Date of Filing 25-Jul-2000
Name of Patentee THE DIRECTOR, FOREST RESEARCH INSTITUTE
Applicant Address P.O. NEW FOREST, DEHRADUN-248 006 INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 PURSHOTTAM LAL SONI FOREST RESEARCH INSTITUTE P.O. NEW FOREST, DEHRADUN-248 006 INDIA.
2 PRADEEP SHARMA FOREST RESEARCH INSTITUTE P.O. NEW FOREST, DEHRADUN-248 006 INDIA.
PCT International Classification Number 609K 8/50
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA