Title of Invention

A WATER PROOFING AND SUPER PLASTICIZER COMPOSITION AND PROCESS THEREOF

Abstract Abstract A waterproofing and super plasticizer composition and process thereof. The present invention relates to a waterproofing and super plasticizer composition and process thereof, hereinafter called Proteckta GL-5(M), wherein the waterproofing and super plasticizer composition comprises component A comprising oligomeric mixture of silane- siloxane and other oil soluble additives in the presence a surfactant, component B having aqueous polymer polycarboxylate mixtures, wetting agents, acticides, sugar, small amount of other plasticizers such as Sodium Lignosulphonate, napthalenesulfonic acid/formaldehyde condensates and sodium gluconate ; cellulose , and aluminates.
Full Text

Field of the invention
The present invention relates to a multipurpose, multifunctional composition for reducing the water absorption ability from concrete , more particularly a waterproofing and super plasticizer composition and preparation thereof, hereinafter called Protekta GL-5(M), which is very effective to imparts hydrophobicity to concrete and reduces the water absorption ability of the concrete by 80-90%.
Background of the invention:
Concrete admixtures are well known and are primarily used to reduce the water cement ratio and increasing its workability for eg salts of napthalenesulfonic acid/formaldehyde condensates (naphthalene derivatives), salts of melaminesulfonic acid / formaldehyde condensates (melamine, derivatives), salts of sulfanilic acid/phenol formaldehyde co-condensates (aminosulfonic acid derivatives), and salts of polycarboxylic acids (polycarboxylic acid derivatives) etc.
The main disadvantage of these admixtures is to react with cement and give rise to undesirable side products and thus affecting the durability of the concrete. More over most of these admixtures are effective only for 30 minutes and after this period they are again added at the site tempering the concrete.
The ready mixed concrete which is recommended to the customers has problem of slump retention, if they continue to use it with readily available admixtures in the market.


However polycarboxyiate products are better since they work on steric hindrance. But they can not be used as admixtures as waterproofing because they are only useful in maintaining water cement ratio.
Concrete is hydrophilic and therefore absorbs water, brings with it lot of toxic materials from the environment like chloride ions, sulphur dioxide, nitrogen dioxide, resins and other materials. When this water finds an ingress point in the concrete id moves in the concrete and disturbs the alkaline passive protection to reinforcement, and causing corrosion.
The only product which is well known as a waterproofing admixture is alkyl or alkaline salts of oleates & stearates and sometimes acrylates.
The main disadvantage of these products are not very effective and do not impart the hydrophobicity to the extent that it really requires and normally since their mechanism of action is based on enteric coating, they are vulnerable to outside factors like calcium hydroxide.
Therefore there is a very critical and urgent requirement of developing a waterproofing admixture which can reduce water absorption of concrete by at least 80 - 90%. These compositions have problems, although each is useful in its own way. Some of the composition react with cement sometimes and give rise to undesirable side products and thus affecting the durability of the concrete. More over most of these admixtures are

effective only for 30 minutes and after this period they are again added at the site thus tempering the concrete.
The ready mixed concrete which is recommended to the customers has problem of slump retention, if they continue to use it with readily available admixtures in the market.
However polycarboxylate products are better since they work on steric hindrance. Any claims to call these compositions as waterproofing is wrong since they are only useful in maintaining water cement ratio. Therefore there is a very critical and urgent requirement of developing a waterproofing admixture which can reduce water absorption of concrete by at least 80 - 90%.
Prior Art
US patent no. 5911820 teaches a concrete admixture comprises a copolymer comprising, as structural units, units derived from an ethylenically unsaturated monomer (a) having 25 to 300 moles of C.sub.2 -C.sub.3 oxyalkylene groups and units derived from a monomer (b) of an alkyl, alkenyl or hydroxyalkyl ester of an ethylenically unsaturated mono- or di-carboxylic acid. Therefore, carboxyl groups which serves as an adsorbing group is gradually increased through hydrolysis of ester with an alkali to result in supplying a freshly formed dispersant, which may be the reason why the fluidity is not loared but maintained for a long period of time. When the copolymer has lengthened side chains by an increase in the mole number of oxyalkylene groups added, it exhibits an enhanced dispersing effect due to steric repulsion and therefore can impart fluidity even

when a reduced amount is used. Therefore, the surface hydration of cement is little hindered to result in a slight retardation of the hardening property.
US patent no. 7,048,793 teaches a compositions for modifying hydratable cementitious materials comprising (A) a lignosulfonic acid or salt thereof; an aldohexonic acid or salt thereof; an hexuronic acid or salt thereof; an hexaric acid or salt thereof; or mixture thereof; and (B) at least one aldopentonic acid or salt thereof.
Patent WO/1995/022580 teaches an aqueous siloxane emulsion comprises: (i) hydrolysable alkylalkoxysiloxane, (ii) 0,1 % to 10 % by weight of a surfactant selected from the group consisting of an alkylamine alkoxylate, or, an acidified or partially acidified alkylamine alkoxylate, quaternary alkyl ammonium salts, acid alkylamine salts and imidazoline salts; and (iii) water. The invention also provides that up to 45 % by weight of the emulsion may be alkylalkoxysilane of the formula: R"n - Si - R"'4-n wherein R" is a hydrocarbyl group containing from 1 to 20 carbon atoms, R"' is a hydrolysable group, and n is 1 or 2. These emulsions maintain high effective levels of the active silicone content on long term storage. The emulsions of the invention are useful in rendering permeable mineral substrates water repellent.
US patent No. 5110684 teaches a method of rendering masonry architectural building materials water repellent by incorporating into the masonry architectural building material an additive comprising (i) a water soluble silane coupling agent and (ii) an emulsion which includes water, at least one surfactant, and a siloxane fluid. The siloxane fluid is one of a linear

methylalkyl siloxane copolymers, methylhydrogen cyclosiloxane polymers, or methylhydrogen-methylalkyl cyclosiloxane copolymers.
Object of the invention:
The main object of the invention is to provide a multifunctional, multipurpose composition, which is very effective to impart hydrophobicity to concrete.
Another object of the invention is to control water cement ratio, because if water is more than 0.3 -0.4, it reduces the compressive strength of the concrete and has adverse effects on the durability and sustainability of the concrete.
Still another object of the invention is to increase the retention of slump for at the least 2 hrs.
Summary of the invention:
The present invention relates to a waterproofing and super plasticizer composition and process thereof, hereinafter called Protekta GL-5(M), wherein the process of making a waterproofing super plasticizer composition comprising the following steps:
a) Taking a surfactant 1 to 5% by w/v in a reactor vessel fitted with an appropriate homogenizer with speed of 2000 to 5000 rpm.
b) Adding water 10 to 20% by w/v.
c) Stirring the solution vigorously till obtaining a homogenous solution.
d) Stirring the said solution with a weak acid vigorously till the solution attains a pH 6 to 7 ,

e) Taking alkyl triethoxy silane and siloxane in another vessel in a ratio of 30 to 80% and 80 to 20% by w/v.
f) Mixing the two by vigorously for 60 to 90 minutes and at the speed of 3000 to 4000 rpm.
g) A gain stirring the solution at speed of at least 2000 rpm for 100 to 140 minutes to obtain a water soluble acrylic polymer hereinafter called Component A.
h) Taking sugar 1 to 6% by w/v and water 20 to 25% by w/v in a reactor vessel
fitted with homogenizer. i) Adding plasticizer 20 to 50% w/v. j) Stirring the said solution 10 to 20 minutes, k) Adding nepthalenesulfonic acid/formaldehyde condenstate 5 to 20% by w/v
and stirring for 10 to 40 minutes. 1) Adding aqueous polymer polycarboxylate solution 20 to 50 % by w/v m) Adding foaming agent to this solution in .5 to 5 % by w/v and acticides .1
to 1 % and stirring the solution for 8 to 10 minutes to obtain component B. n) Taking component B, aluminates along with water in ratio of 1 to 15% by
w/v in to the reaction vessel fitted with homogenizer, stirring 10 minutes, o) Mixing the component A and component B into the ratio of 40 to 80% and 5
to 25% respectively. Thus obtaing a waterproofing super plasticizer
composition.

According to another embodiment of the invention a waterproofing super plasticizer
comprising Component A and component B mixed together with cellulose and
aluminates.
According to another embodiment of the invention component A comprises oligomeric of
mixture of alkyl triethoxy silane and siloxane and other oil soluble additives and
surfactants.
According to another embodiment of the invention component B comprises aqueous
polymer polycarboxylate mixture, wetting agent, aciticides, sugar and plasticizers.
According to another embodiment of the invention the component A and component B are mixed in a ratio of .5 to 5%.
According to another embodiment of the invention the surfactant is ethoxylate or emulsion with cationic or anionic or nonionic or with the combination of cationic, anionic and nonionic.
Detailed description of the invention:
The present invention a waterproofing and super plasticizer composition comprising component A comprising oligomeric mixture of silane- siloxane and other oil soluble additives in the presence a surfactant, component B having aqueous polymer polycarboxylate mixtures, wetting agents, acticides, sugar, small amount of other plasticizers such as Sodium Lignosulphonate, napthalenesulfonic acid/formaldehyde condensates and sodium gluconate ; cellulose , and aluminates.

Component A
Using oligomeric mixture of silane -siloxane and other oil soluble additives in the presence of a surfactant and this solution is stirred using homogenizer at a speed of 3000 -13500 RMP.
Many organic silicones such as alkylalkoxysilanes, alkylalkoxysiloxanes, polysiloxanes can be used (but there are advantages and disadvantages with the choice of each component). While siloxane with large molecular weight achieve early water repellency but it has poor penetration ability due to the higher molecular weight. The advantages of using silanes either neat or dissolved in the solvents give high penetration ability but the volatility of silanes results in poor water repellency. Therefore the best combination is the oligomeric mixture of silanes and siloxanes. This emulsion needs a specific design of surfactant and several combination are tried like
Emulsions or Impregnants
Emulsion with anionic
Emulsion with cationic
Emulsion with mixed cationic & nonionic
Emulsion with acidified amine ethoxylate
Table: 1
Different combination of surfactant systems are used, however the acidified alkylamine ethoxylate surfactants, Oleyl Amine low mole EO, Stearyl Amine low mole EO are found

to be more suitable. These surfactants possess the properties of both cationic and nonionic surfactants and on neutralization with any weak acid preferably acetic acid and a resinous product is formed which is continuously stirred and to this surfactant mix, mixture of silane-siloxane is added drop wise and stirred for 2 hrs. This emulsion is passed through nanometer to achieve a smaller particle sized of the resultant aqueous emulsion.
Component B
Component B is made by mixing aqueous polymer polycarboxylate mixtures, wetting agents, acticides, sugar, small amount of other plasticizers like Sodium Lignosulphonate, napthalenesulfonic acid/formaldehyde condensates and sodium gluconate. This mixture is blended in water and stored as component B
Component A and Component B are mixed together and some amount of cellulose. Aluminates is added to this mix. The resulting product is a waterproofing and super plasticizer composition, called as Protekta GL -5 (M).
According to the invention A process for making a waterproofing super plasticizer composition comprising the following steps: Component A:
(a) Taking a surfactant 1 to 5% by w/v in a reactor vessel fitted with an appropriate homogenizer with speed of 2000 to 5000 rpm.
(b) Adding water 10 to 20% by w/v.

(c) Stirring the solution vigorously till obtaining a homogenous solution.
(d) Stirring the said solution with a weak acid vigorously till the solution attains a PH 6 to7
(e) Taking alkyl triethoxy silane and siloxane in another vessel in a ratio of 30 to 80% and 80 to 20% by w/v.
(f) Mixing the two by vigorously for 60 to 90 minutes and at the speed of 3000 to 4000 rpm.
(g) A gain stirring the solution at speed of at least 2000 rpm for 100 to 140 minutes to obtain a water soluble acrylic polymer hereinafter called Component A.
Component B
(h) Taking sugar 1 to 6% by w/v and water 20 to 25% by w/v in a reactor vessel
fitted with homogenizer. (i) Adding plasticizer 20 to 50% w/v. (j) Stirring the said solution 10 to 20 minutes, (k) Adding nepthalenesulfonic acid/formaldehyde condenstate 5 to 20% by w/v and
stirring for 10 to 40 minutes. (1) Adding aqueous polymer polycarboxylate solution 20 to 50 % by w/v (m) Adding foaming agent to this solution in .5 to 5 % by w/v and acticides .1 to 1
% and stirring the solution for 8 to 10 minutes to obtain component B. A waterproofing and super plasticizer composition
(n) Taking component B, aluminates along with water in ratio of 1 to 15% by w/v
in to the reaction vessel fitted with homogenizer, stirring 10 minutes, (o) Mixing the component A and component B into the ratio of 40 to 80% and 5 to
25% respectively to obtain a waterproofing super and plasticizer composition.

Example 1 Component A
Take a clean and dry stainless steel reactor ranging from 50 to 500 Kg fitted with homogenizer with speed of 2000 to 5000 rpm. 1 to 5 % by w/v of ethoxylate in is taken in the vessel along with the distilled water 10-20% by w/v . This is stirred vigorously and is acidified using a weak acid, the acid is diluted in water 10 to 20 times. The acid solution is added till it gives pH 6 to 7 with continuous stirring. In a separate vessel alkyl triethoxy silane (propyl, butyl, n-butyl, isooctyl, isobutyl), and silicones like polysiloxanes are taken in the 30 to 80% and 80 to 20 % by w/v (thus making total volume as 100) and this mixture is added to the vessel with vigorous stirring (3000 to 4000 rpm) for 60 to 90 minutes and later on stirred at about 2000 rpm for 120 minutes.
This resulted in a water soluble acrylic polymer and during the reaction alchoholic smell may be indicated. It should be ensured that fruity smell comes.
Component B
Take a reactor fitted with a homogeniser. Take water 20 to 35%, sugar 1 to 6%, Sodium Lignosulfonate 25 to 50 % in and stir for 10 to 15 minutes. Add napthalenesulfonic acid/formaldehyde condensates in 5 to 20% ratio and stir for 10 to 18 minutes. Add aqueous polymer polycarboxylate in 20 to 50% ratio and , stir for 5 to 12 minutes. Add foaming agent in 0.5 to 5% ratio and 0.1 to 1% of acticides and stir for 8 to 10 minutes.
12

Take component B, water, aluminates in 1 to 15% ratio into the reaction vessel fitted with homogeniser, stir for 10 min. now mix Component A 40 to 80% & component B 5 to 25%. Add 1 to 4 kg of cellulose fiber, 12.5 kg of continue the stirring over a period of 1 hr.the resultant is a waterproofing and super plasticizer composition Protekta GL-5 (M). 125 gm of this mix is taken in concrete mix containing one bag of cement and the resultant concrete shows the following properties
Reduction in water absorption: 80-90% Compressive strength
7 days 23mpa
28days 42.5mpa
Slump
Ohr : 220 - 260mm
1 hr : 190 - 230mm
2hr : 140 - 170mm
Example 2 Component A
Take a clean and dry 20 ltrs stainless steel reactor fitted with homogeniser. Take 9.6 gm of distilled water in the reactor and add Upanal PT 74 or any other surfactant as given in table 1. Stir it vigorously for one hour. Prepare a solution of 0.5gm of a weak acid in 2.0 gm of distilled water. Add the acid solution drop by drop into the reactor over a period of 15 min, stir for 30min. Prepare a mixture of 12 gms of alkyl triethoxy silane (or any one of the following propyl, n-octyl, isooctyl, isobutyl) add 12 gms of siloxane in it.


Add the above mixture into the reactor drop wise over a period of 1 Vi hour, and then stir the reaction mixture for 2 hrs. Component B
Take a reactor fitted with a homogeniser. Take 450 gm of water, add 250 gm of sodium lignosulfonate, 100 gm of napthalenesulfonic acid/formaldehyde condensates and stir for 15 min. Add 600 gm of aqueous polymer polycarboxylate, stir for 10 min. Add a small amount of biocide, stir for 10 min.
Take 69 gm of component B, 12.5 gm of water, 5 gm of aluminates into the reactor vessel fitted with homogeniser, stir for 10 min. Add 1 to 4 gm of cellulose fiber, 12.5gm of component A and continue stirring over a period of lhr.
300 gm of this mix is taken in concrete mix containing one bag of cement and the resultant concrete shows the following properties
Reduction in water absorption: 80-90% Compressive strength
7 days 23mpa 28days 42.5mpa
Slump
Ohr : 220 - 260mm 1 hr : 190 - 230mm 2hr : 140 - 170mm
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We claim:
1. A process for making a waterproofing and super plasticizer composition, hereinafter called Protekta GL-5 (M), comprising the following steps:
a) Taking a surfactant 1 to 5% by w/v in a reactor vessel fitted with an appropriate homogenizer with speed of 2000 to 5000 rpm.
b) Adding water 10 to 20% by w/v.
c) Stirring the solution vigorously till obtaining a homogenous solution.
d) Stirring the said solution with a weak acid vigorously till the solution attains a PH 6 to7
e) Taking alkyl triethoxy silane and siloxane in another vessel in a ratio of 30 to 80% and 80 to 20% by w/v.
f) Mixing the two by vigorously for 60 to 90 minutes and at the speed of 3000 to 4000 rpm.
g) A gain stirring the solution at speed of at least 2000 rpm for 100 to 140 minutes to obtain a water soluble acrylic polymer hereinafter called Component A.
h) Taking sugar 1 to 6% by w/v and water 20 to 25% by w/v in a reactor vessel fitted with homogenizer.
i) Adding plasticizer 20 to 50% w/v.

j) Stirring the said solution 10 to 20 minutes.
k) Adding nepthalenesulfonic acid/formaldehyde condenstate 5 to 20% by w/v and stirring for 10 to 40 minutes.
1) Adding aqueous polymer polycarboxylate solution 20 to 50 % by w/v
m) Adding foaming agent to this solution in .5 to 5 % by w/v and actinides 0.1 to 1 % and stirring the solution for 8 to 10 minutes to obtain component B.
n) Taking component B, aluminates along with water in ratio of 1 to 15% by w/v in to the reaction vessel fitted with homogenizer, stirring 10 minutes.
o) Mixing the component A and component B into the ratio of 40 to 80% and 5 to 25% respectively to obtain a waterproofing and super plasticizer composition.
2. A process for making a waterproofing and super plasticizer composition as claimed in claim 1, wherein the component A and component B are mixed in a ratio of 0.5 to 5%
3. A process for making a waterproofing and super plasticizer composition as claimed in claim, wherein the component B 50 to 75% by w/v along with 12.5% water and .5 to 5% aluminates is added to reactor vessel fitted with homogenizer, stirring it for 10 minutes and adding 1 to 4% of cellulose fiber and adding 5 to 25% of component A and continuous stirring for at least 1 hour. Thus obtain the waterproofing super plasticizer.
4. A waterproofing and super plasticizer as claimed in claim 1 comprising Component A and component B mixed together with cellulose and aluminates.


5. A waterproofing and super plasticizer as claimed in claim 4, wherein the component A comprises oligomeric of mixture of alkyl triethoxy silane and siloxane and other oil soluble additives and surfactants.
6. A waterproofing and super plasticizer as claimed in claim 5, wherein alkyl triethoxy silane is selected form the group consisting of propyl, n-octal, isooctyl, isobutyl.
7. A waterproofing and super plasticizer as claimed in claim 5, wherein the said
surfactant is ethoxylate or emulsion with cationic, anionic, nonionic or with the
combination of cationic, anionic and nonionic.
8. A waterproofing and super plasticizer as claimed in claim 4, wherein the component B
comprises aqueous polymer polycarboxylate mixture, wetting agent, aciticides, sugar
and plasticizers.
9. A waterproofing and super plasticizer as claimed in claim 8, wherein the said
plasticizer is selected from the group consisting of sodium lignosulphate,
nepthalenesulfonic acid and sodium gluconate.
10. A waterproofing and super plasticizer substantially as hereinbefore described with reference to the accompanying examples.
11. A process for making a waterproofing and super plasticizer composition substantially as hereinbefore described with reference to the accompanying examples.
12. A waterproofing and super plasticizer composition substantially as hereinbefore
described with reference to the accompanying examples.



Documents:

2001-che-2008 abstract.pdf

2001-CHE-2008 AMENDED CLAIMS 16-12-2013.pdf

2001-CHE-2008 AMENDED PAGES OF SPECIFICATION 16-12-2013.pdf

2001-che-2008 claims.pdf

2001-che-2008 correspondence-others.pdf

2001-che-2008 description(complete).pdf

2001-CHE-2008 EXAMINATION REPORT REPLY RECIEVED 16-12-2013.pdf

2001-che-2008 form-1.pdf

2001-che-2008 form-26.pdf

2001-CHE-2008 FORM-3 16-12-2013.pdf

2001-che-2008 form-3.pdf

2001-CHE-2008 FORM-5 16-12-2013.pdf

2001-che-2008 form-5.pdf


Patent Number 258689
Indian Patent Application Number 2001/CHE/2008
PG Journal Number 06/2014
Publication Date 07-Feb-2014
Grant Date 31-Jan-2014
Date of Filing 18-Aug-2008
Name of Patentee TECH-DRY (INDIA) PVT. LTD
Applicant Address 769, GROUND FLOOR, 1ST STAGE, 1ST CROSS, INDRA NAGAR, BANGALORE-560 038
Inventors:
# Inventor's Name Inventor's Address
1 SURENDRA P. BHATNAGAR 205, 2ND FLOOR, KRISHNA JEE, 3RD MAIN DEFENCE COLONY, INDRA NAGAR BANGALORE-560 038
PCT International Classification Number C04B24/16; C04B24/26;
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA