Claims:We Claim
1. A wood preservative formulation comprising anti-borer, anti-fungal and termicidal activity comprising coconut shell pyrolytic oil distillate (CSPOD) and inorganic/ metal ions.

2. A wood preservative formulation as claimed in claim 1, wherein the coconut shell pyrolytic oil distillate (CSPOD) is obtained from distillation of coconut shell pyrolytic oil (CSPO).

3. A wood preservative formulation as claimed in claim 1, wherein inorganic/ metal ions are copper ions comprising 1-10% of the total weight of the formulation.

4. A wood preservative formulation as claimed in claim 2, wherein the coconut shell pyrolytic oil is obtained by pyrolysis of coconut shells.

6. A process for formulation of the wood preservative from Coconut Shell pyrolytic oil (CSPO) comprising of steps:
distillation of Coconut Shell pyrolytic oil (CSPO) to obtain the distillate of CSPO (CSPOD);
refluxing of CSPOD with 5-15% copper sulphate (CuSO4) solution for 4-8 hours; and
separating the CSPOD with 1-10% copper content.

7. The formulation as claimed in claim 1, wherein the formulation is used as a termicidal, anti-borer and anti-fungal agent, alone or together with other conventional termicidal and insecticidal agents.

8. A method of protecting wood comprising treating or impregnating the wood with the wood preservative formulation of claim 1.

9. The method of protecting wood as claimed in claim 8, wherein the treating or impregnating comprises pressure application, dipping, rolling, painting, and combinations thereof. , Description:FIELD OF INVENTION
The present invention provides a wood preservative formulation from coconut shell pyrolytic oil. Moreover, the present invention relates to efficient and environmental friendly wood preservative formulation from coconut shell pyrolytic oil. Further, the present invention relates to from coconut shell pyrolytic oil wood preservative with antifungal, anti-borer and anti-termite activity.

BACKGROUND OF INVENTION
Wood is a major forest product and continues to be an extensively used raw material for diverse domestic, industrial and structural applications. It being a natural product is highly prone to attack by insects, mould, fungi, depending on the moisture content of the wood. Principal organisms causing wood decay are insects, fungi, bacteria and termites. The combined activity of the insects and organisms primarily causes immense material loss as well as loss of the resources. There is tremendous need to effectively conserve wood which has been achieved by wood preservatives. Nonetheless, most of the wood preservatives are chemicals or synthetic in nature causing severe environmental and water pollution, eradication of species of microorganisms beneficial to the nature, causing pest resistance etc., Conventional proprietary wood preservatives like CCA (Copper Chrome Arsenic) other synthetic preservatives are detrimental to the environment.

Existing wood preservatives are mainly chemicals that cause a negative impact on environment.

US20100273655 discloses a herbicidal blend having from a) about 0.3 to about 4 parts by volume of a herbicide; b) from about 5 to about 20 parts by volume of a modified plant oil; and c) from about 5 to about 20 parts by volume of a compostable organic particulate. A method for preparing the herbicidal blend and a method of using the blend is also disclosed. The herbicidal blend is effective in controlling invasive water plant flora such as duckweed, water meal and parrot feather. It is prepared from coconut shell and other plant nut shell oils in combination with copper as herbicide.

CA2569813 discloses novel materials for controlling molluscs, such as snails and slugs using carbohydrates including celluloses, hemi-cellulose complexes, and/or lignin, for inducing death in molluscs. The invention discloses carbohydrates derived from plant nut shell like coconut in combination with inorganic compounds like copper salts for use in controlling molluscs.
US5538670 discloses a method for protecting wood against decay and similar degradation reactions caused by wood decay fungi and similar microorganisms which cause wood decay, comprising treating wood with a wood preservative solution containing at least one complexing agent.

US20140017506 discloses wood preservative compositions containing surfactants or phospholipids, methods of applying such wood preservative compositions to wood, and wood products resultant from some such methods. The patent discloses a 2-amino-N,N-dimethylacetamide surfactant and phospholipids for improving wood preservation.

Natural anti-termite formulation using cashew nut shell oil has been disclosed in research articles earlier (Mwalongo, G.C.J., Mkayula, L.L., Mubofu, E.B. and Mwingira, B.A., Environmentally friendly chemical combinations of cashew nut shell liquid, sulfited wattle tannin and copper(II) chloride, Green Chemisty, Vol 35, pp 13-16 (1999); Natural cashew nut shell liquid and neem oil as wood preservative are also disclosed earlier (Nagaveni, C H, Evaluation of copperised cashew nut shell liquid and neem oil as wood preservatives [J], 2018).

Aforesaid prior art discloses wood preservative compositions which are chemical agents or surfactants or from natural derivatives where further research is required. There is a need for safe, easy to apply, wood protectant that protects wood against wood destroying agents. Commercially available and earlier disclosed wood preservative compositions or formulation have a major disadvantage of being toxic and irritating to humans. It will be advantageous to develop natural wood preservative that is environmental friendly and acceptable. Therefore, the development of alternative control measure against wood destroying agents for an eco-friendly environment is highly essential. Keeping view on this point, it is urgently required to prepare a safe, eco-friendly biological based wood preservative formulation that is easily available as a natural resource and imparts protection against wood destroying organisms.

Accordingly there is a necessity to develop a natural wood preservative formulation which is nontoxic, eco-friendly and biodegradable in the environment with no adverse effects.

OBJECTS OF THE INVENTION
It is a primary object of the invention to provide an efficient, environmental friendly, cost-effective wood preservative formulation from the coconut shell pyrolytic oil.

It is another object of the present invention to provide wood preservative formulation from coconut shell pyrolytic oil for both indoor and outdoor applications.
It is another object of the present invention to provide wood preservative formulation from coconut shell pyrolytic oil distillate.

It is a further object of the present invention to provide a wood preservative formulation from coconut shell pyrolytic oil comprising CSPOD and inorganic or metal ions, wherein the metal ions are copper ions at a concentration of 1-10% of the total weight of the formulation.

It is a further object of the present invention to provide a wood preservative formulation from coconut shell pyrolytic oil for protection of wood against wood destroying agents like wood borer, termites and wood decay fungi.

It is a further object of the present invention to provide a process for formulation of the wood preservative from the coconut shell pyrolytic oil.

It is another object of the present invention to determine the termicidal, fungicidal, anti-borer efficacy of the formulation using standard tests.

SUMMARY OF INVENTION
Thus, the basic aspect of the present invention is to provide a natural wood preservative with anti-borer, anti-fungal and anti-termite activity.
It is another aspect of the present invention to provide a wood preservative formulation with anti-borer, anti-fungal and termicidal activity comprising coconut shell pyrolytic oil distillate (CSPOD) and inorganic/ metal ions.

It is another aspect of the present invention to provide a wood preservative from coconut shell pyrolytic oil distillate (CSPOD), wherein the distillate is obtained from distillation of coconut shell pyrolytic oil (CSPO).

It is another aspect of the present invention, wherein the coconut shell pyrolytic oil distillate (CSPOD) formulation comprises 1-10% of the total weight of the formulation of metal or inorganic ions.

It is another aspect of the present invention, wherein the coconut shell pyrolytic oil is obtained by pyrolysis of coconut shells.

It is another aspect of the present invention to provide a process for formulation of the wood preservative from Coconut Shell pyrolytic oil (CSPO) comprising of steps:
distillation of CSPO;
collection of distillate of CSPO (CSPOD);
refluxing of CSPOD with 5-15% copper sulphate (CuSO4) solution for 4-8 hours; and
separating the CSPOD with 1-10% copper content.

It is another aspect of the present invention, wherein the CSPOD formulation is used as a termicidal, anti-borer and anti-fungal agent, alone or together with other conventional termicidal and insecticidal agents.

It is another aspect of the present invention, wherein the wood protection or preservation is imparted to the wood by either treating or impregnating the wood with the wood preservative formulation.

It is yet another aspect of the present invention, wherin treating or impregnating comprises pressure application, dipping, rolling, painting, and combinations thereof.

BRIEF DESCRIPTION OF THE DRAWINGS:
Further objects and advantages of this invention will be more apparent from the ensuing description when read in conjunction with the accompanying drawings, wherein:
Figure 1: illustrates the chemical composition of CSPOD determined using GC-MS analysis
Figure 2: illustrates antifungal study as per BIS standards 4873 (Part I:2008)
Figure 3: illustrates anti-termite study as per IS 4833:1993 (Accelerated field tests)
Figure 4: illustrates termicidal activity of the formulation in comparison with commercial wood preservative as per IS4833:1993 (Accelerated field tests)

DETAILED DESCRIPTION OF THE INVENTION
The present disclosure generally relates to wood preservatives and methods of treating wood. More particularly, the wood preservatives and methods of treating wood include applying to the wood, a wood preservative composition comprising coconut shell pyrolytic oil. In a preferred embodiment the wood preservative composition comprises coconut shell pyrolytic oil distillate with inorganic or metal ions.

Wood is an important natural resource and finds application in as building material of choice in a vast variety of applications, especially as a raw material in domestic, industrial and structural application. Being a natural material it is subject to deterioration by some principal organisms like insects, fungi, bacteria, and termites. Wood generally is subject to rapid deterioration when wet or moist; and wood exposed to the elements is commonly treated to retard deterioration. Destruction of the wood generally is caused by insects, mold, fungi, termites, borer and a vast variety of microorganisms. Although there are a plethora of chemical agents that impart protection and preservation of wood, it leads to environmental pollution and water pollution and death of beneficial species. The conventional proprietary wood preservatives such as Copper chrome Arsenic or CCA, Copper Chrome Boron or CCB, are under scrutiny due to environmental reasons. Hence wood is to be protected with thoroughly biodegradable substances, so that the treated wood has a useful and safe life cycle and disposal. Current research focuses on wood protection using natural environmentally compatible compounds.

Coconut trees are grown in large numbers in India and many South Asian countries and coconut shells are available in large quantities. The coconut shells are largely used as a fuel and to certain extent in handicrafts industry. Coconut shells are used as fuels and gasifier and coconut shell pyrolytic oil is produced as a by-product. Coconut shells are burnt (incomplete combustion) under limited supply of air (30%) at temperature of 950°C-1000°C to generate producer gases and coconut shell pyrolytic oil, which is dark thick liquid collected at the bottom of the gasifier. Generally, coconut shell pyrolytic oil is a by-product of charcoal industry, which otherwise has little value except as a fuel oil dilute in India. Therefore its utilization as wood would preservative will expand the reach of such industries by increasing their operations and income sources.

A good wood protectant should protect wood from all the wood deteriorating agents namely wood decay fungi, termites and borers. The present invention is a result of extensive research on natural wood preservative whose wood-preserving efficacy is superior to that of conventional wood preservatives.

Generally, coconut shell pyrolytic oil is a by-product of charcoal industry, which would otherwise have little value except as a fuel oil dilute in India. Therefore its utilization as wood would preservative will expand the reach of such industries by increasing their operations and income sources.According to the present invention, there is provided wood preservative comprising coconut shell pyrolytic oil. In a preferred embodiment of the present invention is provided a wood preservative composition or formulation comprising Coconut shell pyrolytic oil distillate.

A good wood protectant should protect wood from all the wood deteriorating agents namely, wood decay fungi, termites and borers. Therefore, to assess the efficacy of coconut shell pyrolytic oil as a wood protectant, anti-borer, anti-fungal and termicidal activity of coconut shell pyrolytic oil was explored as per BIS standards. The results indicated that coconut shell pyrolytic oil imparts significant protection against the wood deteriorating agents both in laboratory and field conditions. Since coconut shell pyrolytic oil is a dark viscous liquid, it can be recommended only for outdoor applications. To improve the efficacy and aesthetic value of the coconut shell pyrolytic oil further, it was modified by various methods to get different fractions. Coconut shell pyrolytic oil is a dark viscous liquid which imparts significant protection against wood deteriorating agents. Coconut shell pyrolytic oil is subjected to distillation to get coconut shell pyrolytic oil distillate (CSPOD). This is achieved by subjecting the coconut shell pyrolytic oil to distillation using Dean and Stark Apparatus. TO CSPOD or the distillate, is added 5-15% copper sulphate solution CUSO4 and refluxed for 4-8 hours. This gives the final distillate or CSPOD with 1-10% copper content. Since metal ions are prone to leaching, the effectiveness of the formulation was further improved by linseed coating. Finally the most effective formulation was compared with the commercially available wood preservatives and found to be very efficient.

Out of all the fractions CSPOD or Coconut shell pyrolytic oil distillate is a colorless liquid with improved aesthetic value and efficacy. Compositional analysis for identification of the active compounds of the CSPOD was done using Gas chromatography-mass spectroscopy (GC-MS) (thermo Scientific, Trace GC Ultra MS: DQII). Analysis of sample was done with electron Impact Ionization for MS using Quadrupole mass analyser. Efficacy of the CSPOD is further improved by introducing inorganic ions and plant extracts and oils. The CSPOD composition was deciphered using GC-MS and the compositional analysis is given in table 1.
Table 1:
Peak No RT (min) Name of compound
1 10.51 Phenol
2 11.67 o-cresol
3 12.03 p-cresol
4 12.3 o-Guaiacol
5 13.91 p-creosol
6 15.17 p-Ethylguaiacol
7 16.20 Syringol
8 17.48 Benzene, trimethoxy
9 18.44 Dodecanoic acid, methyl ester
10 18.49 5-tert-Butyl-1,2,3-benzenetriol

As illustrated in Figure 1, the major component of coconut shell pyrolytic oil distillate is found to be phenol (peak 1) and phenolic compounds.
According to a one embodiment of the present invention coconut shell pyrolytic oil produced as a result of pyrolysis of coconut shell has shown potential anti-fungal activity against wood decay fungi.

The coconut shell pyrolytic oil distillate was evaluated for the antifungal activity, anti-borer activity and Termicidal activity.

Specimen and treatment methods
Specimens were made of Rubber wood (Hevea brasiliensis). Rubber wood has a density of 560~640 kg/m3 (16% M.C.). It comes under non-durable class of timber. The samples selected for the study were free from visual defects.
Rubber wood test blocks of size 1.9X1.9X1.9cm with long axis parallel to the grain of the wood are prepared from rubber wood, free from knots, moulds and stains were used for antifungal study.
Rubber woodblocks tested positive for starch reserves is used for anti-borer study. The test blocks of size 5.0 x 2.5 x 1.5cm with long axis parallel to the grain of the wood are prepared from rubber wood, free from knots, moulds and stains. Each block is then tested for starch content and weighed.
Rubber wood stakes of 15.3X3.8X0.625 cm for accelerated study with long axis parallel to the grain of the wood free from insect or fungal attack were air seasoned to constant weight and used for anti-termite study. Wood blocks were numbered and kept in the over at 102±30°C for 48 hrs and weighed. The weighed blocks were then placed in desiccators.
I - Spraying (Brush coating) method– The treatment solution shall be sprayed over the test specimens uniformly. II- Dipping method – The test specimens shall be dipped in the treatment solution for 48 hours. III - Pressure impregnation method- Impregnation of treatment solution for 15 minutes of vacuum, 60 minutes of 50psi pressure shall be given during this method of treatment. Six replicates of test specimens (wood blocks) are used for each method. The six untreated wood blocks served as controls.

Antifungal study as per BIS standards IS 4873 (Part I of 2008)
Culture of test fungi Trametes hirsute Wulf. ex Fr.(white rot) bearing FRI number FRI No. 534 and Polyporus meliae (Undrew.) Murrill (brown rot) bearing FRI number 836 which are one week old and virulent were used. The authentic cultures of these fungi were procured from National Type Culture Collection, Dehradun, India and maintained at Institute of Wood Science and Technology, Bengaluru. Treated wood blocks were introduced aseptically in to the bottles having actively growing fungal culture. Two wood blocks per bottle were kept on glass rings placed inside the bottles. Culture bottles containing the wood blocks were incubated at room temperature (25 ± 1 °C) at 70 ± 4% RH. The wood blocks were harvested after 16 weeks, autoclaved, brushed off fungal mat and oven dried to constant weight before being weighed (W2). Weight loss percentage (WL) of samples after fungal exposure was calculated as follows:
%WL = [(W1 – W2)/ W1] X 100
Where W1 is the oven-dry weight of sample prior to exposure and W2 is the oven-dry weight of sample after exposure to fungus.

Table 2: Mean percentage weight losses of coconut shell pyrolytic oil distillate treated samples exposed to wood decay fungi.
Treatment Fungus (average weight loss percentage )
Polyporus meliae (Undrew.) Murrill Brown rot Trametes hirsute Wulf. ex Fr White rot
Control 29.37 39.29
CSPOD- brush coating 13.56 30.18
CSPOD- dip treatment 10.59 13.07
As illustrated in Table 2 and figure 2 the weight loss due to fungal exposure was significantly reduced in wood blocks treated with CSPOD when compared with the untreated blocks. Dip treated wood blocks showed more resistance to fungal attack on treatment with CSPOD compared to brush coated blocks.

Anti-borer study of the formulation as per BIS standards IS 4873 (Part II: 2008)
BIS standards IS 4873 (Part II: 2008) was used for anti-borer study. Six blocks per each concentration, six untreated control blocks and six treated with the solvent alone were exposed individually to six pairs of freshly emerged Lyctus africans Lesne adult beetles. The activities of the beetle were indicated by the presence of powder like dust thrown out (frass) (Adult release method). Observations are continued until adult beetles emerge from the test specimens. The exit holes visible in control blocks indicated completion of the L. Africans life cycle and emergence of new generation. There were no exit holes in the treated test blocks. As illustrated in Table 3 the wooden blocks were evaluated based on presence or absence of exit holes in the wooden blocks.
No of months
After exposure

Treatment 3 6 9 12 15 18 21 24
Brush Coating NEH NEH NEH NEH NEH NEH NEH NEH
Dip Coating NEH NEH NEH NEH NEH NEH NEH NEH
Control NEH NEH EHA EHA EHA MEHA MEHA MEHA
Table 3: Anti-borer study as per BIS Standards IS 4873 (Part II:2008)
Average of six replicates,
NEH-No exit holes
EHA- Exit holes appeared
MEHA- More exit holes appeared

As illustrated in table 3 the wooden blocks treated with the CSPOD formulation showed no exit holes at the end of 2 years, with both brush treatment and dip treatment.
Anti-Termite Study:
BIS Standard IS 4833 (1993) (Accelerated Grave yard test).
Six replicates of test specimens were used for each method. The six untreated wood blocks served as controls. The air dried treated and control stakes were implanted in the soil at termite test yard following a completely randomized design. All the stakes were half buried in rows and a distance of one foot was maintained between the stakes. The surrounding soil was firmly pressed around the stakes to ensure good contact with the soil.
After two year of field evaluation it was observed that CSPOD or coconut shell pyrolytic oil distillate formulation significantly protected the treated blocks from termites when compared to untreated control blocks. As illustrated Table 4 and figure 3, the stakes when compared after treatment with the formulation of the present invention using both brush coating and dip coating compared to control, the pressure treatment and dip treatment results indicate higher efficiency compared to brush coating.
Table 4:

Comparison of termicidal activity of the formulation with commercial wood preservatives as per IS 4833:1993 (Accelerated field test)
The efficacy of the formulation was compared to the commercially available wood preservatives as per BIS by a field assay. The termicidal activity of the formulation was compared to Biflex (synthetic origin) and Wudcare (natural origin-CSNL based). As illustrated in figure 4 and table 5 the formulation of the present invention shows improved wood protectant activity in terms of termicidal activity tested on treated rubber wood stakes of Hevea brasiliensis (Willd. Ex. Adr. Juss) for 2 years under field conditions. The results are illustrated in table 5, with data on anti-termite activity of the formulation compared to commercial wood preservatives.

Table 5: