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Patent 1099853 Summary

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(12) Patent: (11) CA 1099853
(21) Application Number: 301244
(54) English Title: WATER SOLUBLE PENTACHLOROPHENOL AND TETRACHLOROPHENOL WOOD TREATING SYSTEMS
(54) French Title: PENTACHLOROPHENOL SOLUBLE DANS L'EAU ET SYSTEMES DE TRAITEMENT DU BOIS A BASE DE TETRACHLOROPHENOL
Status: Expired
Bibliographic Data
(52) Canadian Patent Classification (CPC):
  • 6/13.5
(51) International Patent Classification (IPC):
  • C09D 5/14 (2006.01)
  • B05D 7/06 (2006.01)
  • B27K 3/00 (2006.01)
  • B27K 3/50 (2006.01)
  • B27K 3/52 (2006.01)
(72) Inventors :
  • AMUNDSEN, JOSEPH (United States of America)
  • GOODWIN, ROBERT J. (United States of America)
  • WETZEL, WILLIAM H. (United States of America)
(73) Owners :
  • REICHHOLD CHEMICALS, INC. (United States of America)
(71) Applicants :
(74) Agent: SMART & BIGGAR
(74) Associate agent:
(45) Issued: 1981-04-28
(22) Filed Date: 1978-04-17
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
857,035 United States of America 1977-12-02

Abstracts

English Abstract



ABSTRACT OF THE DISCLOSURE

This invention relates generally to water soluble wood
treating compositions and methods for the preservation of wood or
products made from wood. In the general practice of this inven-
tion, wooden objects are treated with water soluble compositions
comprising blends of (A) from about 0.1% to about 50% by weight
of a chlorophenol selected from a group consisting of pentachloro-
phenol and tetrachlorophenol and mixtures thereof (B) from about
2% to about 98% by weight aliphatic alcohols selected from the
group consisting of N-butyl alcohol, secondary butyl alcohol, iso-
butyl alcohol, tertiary butyl alcohol and isopropyl alcohol and
mixtures thereof (C) from about 0.56% to about 45% by weight of
ammonium hydroxide or an amine selected from the group consisting
of triethyl amine, trimethyl amine, methyl amine and methyldieth-
anol amine and mixtures thereof (D) from about 1% to about 97% by
weight water and (E) from 0% to about 20% by weight sodium hydr-
oxide. In addition, these wood treating formulations may include
varying amounts of tetrasodium pyrophosphate (0-10% by weight),
copper salts (0-10% by weight), sodium chromates (0-10% by weight),
sodium gluconate (0-10% by weight), sodium citrate (0-10% by
weight), sodium N-dihydroxyethylglycinate (0-10% by weight) and
ammonium or sodium lignin sulfonate (0-20% by weight) as added
ingredients. In the practice of our invention, these compositions
are incorporated into treating systems that adequately penetrate
wood and deposit essentially non-leachable chlorophenols in the
wooden objects.


Claims

Note: Claims are shown in the official language in which they were submitted.


THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:

1. Water soluble wood treating and preserving solutions
consisting of blends of (A) from about 0.1% to about 50% by
weight of a chlorophenol selected from a group consisting of
pentachlorophenol and tetrachlorophenol and mixtures thereof
(B) from about 2% to about 98% by weight aliphatic alcohols
selected from the group consisting of N-butyl alcohol, secondary
butyl alcohol, isobutyl alcohol, tertiary butyl alcohol and iso-
propyl alcohol and mixtures thereof (C) from about 0.56% to about
45% by weight of ammonium hydroxide or an amine selected from the
group consisting of triethyl amine, trimethyl amine, methyl amine
and methyldiethanol amine and mixtures thereof (D) from about 1%
to about 97% by weight water and (E) from 0% to about 20% by
weight sodium hydroxide.


2. Water soluble wood treating and preserving solutions
consisting of blends of (A) from about 0.1% to about 50% by weight
of a chlorophenol selected from a group consisting of pentachloro-
phenol and tetrachlorophenol and mixtures thereof (B) from about
2% to about 98% by weight aliphatic alcohols selected from the
group consisting of N-butyl alcohol, secondary butyl alcohol,
isobutyl alcohol, tertiary butyl alcohol and isopropyl alcohol
and mixtures thereof (C) from about 0.56% to about 45% by weight
of ammonium hydroxide or an amine selected from the group consist-
ing of triethyl amine, trimethyl amine, methyl amine and methyl-
diethanol amine and mixtures thereof and (D) from about 1% to
about 97% by weight water.
3. The water soluble wood treating and preserving solutions
according to claim 2 wherein at least one member selected from
the following group is added: tetrasodium pyrophosphate, copper
salts, sodium citrate, sodium n-dihydroxyethylglycinate, ammonium




lignin sulfonate and sodium lignin sulfonate.


4. Water soluble wood treating and preserving solutions
consisting of blends of (A) from about 0.1% to about 50% by
weight of a chlorophenol selected from a group consisting of
pentachlorophenol and tetrachlorophenol and mixtures thereof (B)
from about 2% to about 98% by weight aliphatic alcohols selected
from the group consisting of N-butyl alcohol, secondary butyl
alcohol, isobutyl alcohol, tertiary butyl alcohol and isopropyl
alcohol and mixtures thereof (C) from about 0.56% to about 45%
by weight of ammonium hydroxide or an amine selected from the
group consisting of triethyl amine, trimethyl amine, methyl amine
and methyldiethanol amine and mixtures thereof (D) from about
1% to about 97% by weight water and (E) from 0.02% to about 20%
by weight sodium hydroxide.


5. The water soluble wood treating and preserving solutions
according to claim 4 wherein at least one member selected from
the following group is added: tetrasodium pyrophosphate, copper
salts, sodium citrate, sodium n-dihydroxyethylglycinate, ammonium
lignin sulfonate and sodium lignin sulfonate.

21

Description

Note: Descriptions are shown in the official language in which they were submitted.


;;3

Wood has been used for many years as an importank building and
construction material and its importance as such is increasing for a number
of reasons. Typical uses include general construction, residential housing,
utility poles~ cross arms, fence posts, railroad ties and pilings. Although
wood is a renewable natural resource, it must be protected from attack by
insects and fungus and marine organisms for many of these applications- Left
unprotected or unpreserved, wood will decay and deteriorate anywhere from a
few months to a few years, depending upon climate and soil conditions. Wood
objects such as utility poles and timbers deteriorate rapidly below the ground
and at ground level and would require frequent replacement if not properly
and adequately preserved with a material which is both effective against
attacking organisms and long lasting.
Through the years, a number of different materials have been used
for preservation. Among these are included creosote, heavy metal salts,
heavy oils and tars, pitch and various organic materials including chlorinated
phenols, especially pentachlorophenol (PC~. Each of these materials has its
advantages and disadvantages. Creosote, as well as other heavy oils and tars
and pitch treatments, may have a strong odor and leave the surface greasy
and oily to the touch.
Chlorinated phenols have found wide use because of their effectiveness~
relative ease of application and durability. Because of its particularly
good fungicidal and insecticidal properties, pentachlorophenol is widely used
as a commercial wood preser~ative. It is normallg dissolved in hydrocarbon
solvents such as medium aromatic oils, volatile petroleum solvents (propane),
light solvents (mineral spirits~ or in a chlorinated hydrocarbon solvent-
inhibited grade of methglene chloride. Co-solvents are added in many instances
to achieve proper solubility of pentachlorophenol in the solutions. Because
energy conservation is becoming increasingly important, mc~ny of the traditioncil

treating solvents are more valuable as feed stocks for other chemical products.
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3S3

Therefore, a low energy based solvent such as water has been sought as a
replacement for these hydrocarbon solvents. The difficulty has been that
pentachlorophenol in a simple admixture with water has little or no solubility.
Prior art shows that pentachlorophenol can be reacted with sodium hydroxide
in water to form the water soluble sodium pentachlorophenate. To da~e this
is the only aqueous soluble form of pentachlorophenol that has been commonly
used in the wood treating industry. However, sodium pentachlorophenate
treating solution has a severe disadvantage in its excess leachability during
field use. In the practice of our invention, new water soluble pentachloro-

phenol, treating solutions are disclosed which overcome these problems even
when using sodium pentachlorophenate.
In accordance with this invention, novel pentachlorophenol-aliphatic
alcohol-amine or ammonia systems or tetrachlorophenol-aliphatic alcohol-amine
or ammonia systems are disclosed that areaomF~tible with water and are
soluble therein. Aliphatic alcohols and particularly the butyl alcohols are
essential ingredients in solubilizing pentachlorophenol in water even though
the butyl alcohols are sparingly water sbluble themselves. Volatile amine
or ammonia systems are also essential in providing stability and ePfective
penetration oP the systems into the wood. Upon contact and penetration into
cellulosic materials and during the drying process, the preservative becomes
fixed. It has also been found that when soluble metals such as copper sulphate
or copper carbonate and chromium salts are included in these treating sys~ems,
additional fixation and preservative properties are obtained. In addition,
we have Pound that additives such as tetrasodium pyrophosphate, sodium
gluconate, sodium citrate, sodium N-dihydroxyethylglycinate and a lignin
sul~onate such as ammonium or sodium lignin sulfonate provide increased
effectiveness. In the various Pormulations, water in widely varying percent-
ages is used as themain solvent.
The pentachlorophenol employed in the present compositions may be



-- 2 --




- . . .

~i3

present in pure form or as a technical mix.ture. Pentachlorophenol meeting
the requirements of Federal Specification TT-W-570 and American Wood
Preservers Association P8-7~ is especially suitable. These specifications
require that pentachlorophenol contain not less than 95% of chlorinated
phenols. It shall contain not more than 1~ of matter insoluble in N/l aqueous
sodium hydroxide solution, and it shall have a free~ing point of not less
than 17~ C.
Other chlorinated phenols such as tetrachlorophenol or mixtures of
tetra ~nd pen~achlorophenol may also be used in place of the pentachlorophenol

as we~l as the sodium salts of these chlorinated phenols.
Several things must be considered when attempting to prepare water
soluble pentachlorophenol treating solutions. Acceptable aqueous pentachloro-
phenol treating solutions must be capable of penetrating deep into the wood
and becoming deposited therein in an essentially non-leachable form. Prev-
ious attempts to prepare water soluble pentachlorophenol treating solutions
could not achieve satisfactory results in either of these ~wo requirements.
Therefore, it was unexpected that water soluble pentachlorophenol
treating solutions could be obtained which, in fact, do penetrate deeply into
wood and deposit the pentachlorophenol in an essentially non-leachable form
in the practice of our invention. These solutions generally comprise
pentachlorophenol, a butyl alcohol, an amine or ammonia and water as a solvent.
When wood is pressure treated with such a solution and dried9 the pentachloro-
phenol becomes fixed into the wood.
The unexpected discovery of the effectiveness of aliphatic alcohols,
especially the butyl alcohols in promoting the solubility of pentachlorophenol
into aqueous systems is unique in consideration of the fact that pentachloro-
phenol itself is very insoluble in water and that n-butyl alcohols are only
soluble in water at room temperature to the extent of 9 parts alcohol in ]00
parts water.
-- 3 --

9~3~i3

It was further discovered that the aliphatic alcohol-
pentachlorophenol-amine or ammonia water soluble systems could be
enhanced by pH control and by additions of further additives.
Mixtures of various alcohols can be used successfully
in low amounts in the formulations of our invention as well as
the specific alcohols alone. Among the alcohols used alone or
in combination as a formulation aid are n-butyl alcohol, isopro-
pyl alcohol, n-propanol, allyl alcohol, secondary butyl alcohol,
isobutyl alcohol and tertiary butyl alcohol.
Varying kinds of amines were discovered to be effective
in the formulations; preferably the volatile ones. These include
various concentrations of ammonia water (ammonium hydroxide)
triethyl amine, trimethyl amine, methyl amine, methyldiethanol~
amine and blends of these amines.
Copper salts which may be used include copper sulfate,
copper carbonate, copper hydroxide, copper oxide and copper
chloride. ~ -
According to the first embodiment of the invention there
is provided water soluble wood treating and presert~ing solutions
consisting of blends of (A) from about 0.1% to about 50% by weight
of a chlorophenol selected from a group consisting of pentachloro-
phenol and tetrachlorophenol and mixtures thereof (B) from about
2% to about 98% by weight aliphatic alcohols selected from the
group consisting of N-butyl alcohol, secondary butyl alcohol,
isobutyl alcohol, tertiary butyl alcohol and isopropyl alcohol
and mixtures thereof (C) from about 0.56% to about 45% by weight
of ammonium hydroxide or an amine selected from the group consist-
ing of triethyl amine, trimekhyl amine, methyl amine and methyl-
diethanol amine and mixtures thereof (D) from about 1% to about
97% by weight water and (E) from 0% to about 20% by weight sodium
hydroxide.

According to the second embodiment of the invention -there



-4-
J

8~3
is provided water soluble wood treating and preserving solutions
consisting of blends of (A) from about 0.1% to about 50% by
weight of a ch]orophenol selected from a group consisting of
pentachlorophenol and tetrachlorophenol and mixtures thereof (B)
from about 2~ to about 9~% by weight aliphatic alcohols selected
from the group consisting of N-butyl alcohol, secondary butyl
alcohol, isobutyl alcohol, tertiary butyl alcohol and isopropyl
alcohol and mixtures thereof (C) from about 0.56% to about 45%
by weight of ammonium hydroxide or an amine selected from the
group consisting of triethyl amine, trime-thyl amine, methyl amine
and methyldiethanol amine and mixtures thereof and (D) from about
1~ to about 97% by weight water.
According to the third embodiment of the invention there
is provided water soluble wood treating and preserving solutions
consisting of blends of (A) from about 0.1% to about 50% by
weight of a chlorophenol selected from a group consisting of
pentachlorophenol and tetrachlorophenol and mixtures thereof (B)
from about 2% to about 98% by weight aliphatic alcohols selected
from the group consisting of N-butyl alcohol, secondary butyl
alcohol, isobutyl alcohol, tertiary butyl alcohol and isopropyl
alcohol and mixtures thereof (C) from about 0.56% to about 45%
by weight of ammonium hydroxide or an amine selected from the
group consisting of -triethyl amine, trimethyl amine, methyl amine
and methyldiethanol amine and mixtures thereof (D) from about 1%
to about 97% by weight water and (E) from 0.02% to about 20% by
weight sodium hydroxide.
In addition, these wood treating formulations may
include varying amounts of tetrasodium pyrophosphate (0-10% by
weight), copper salts (0-10% by weight), sodium citrate (0-10%
by weight~i sodium N-dihydroxyethylglycinate (0-10% by weight)and
a lignin sulfonate such as ammonium or sodium lignin sulfonate
(0-20% by weight) as added ingredients.




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53
As stated previously, extreme leachabili-ty problems
have always been encountered when using water solutions of sodium
salts of chlorinated phenols as wood preservatives. By practice
of our invention it is now possible to prepare water-borne solu-
tions of sodium pentachlorophenate and tetrachlorophenate which
may be deposited in wood in essentially a non-leachable form.




-4b-


,

s~

Either pentachlorophenol or tetrachlorophenol may be used and formed
into the sodium salt prior to use by reacting with sodium hydroxide or
previously prepared commercially available sodium pentachlorophenate or
tetrachlorophenate may be used.
If pentachlorophenol or tetrachlorophenol are used as the starting
material they are mixed with sodium hydroxide and water. Then the treating
solution is prepared from copper sulfate, an amine or ammonia and a lignin
sulfonate. In this marmer, a ~reating solution is prepared which, when used
to treat the wooden objects of this in~ention, deposits the chlorophenate in
the wood in an essentially non-leachable form. Any of the amine, ammonia or
lignin sulfonates previously described may be used. It has been found that
solutions may be prepared using from about 0.1% to about 50% by weight
pentachlorophenol or tetrachlorophenol, from about 0.02% to about 20% by
weight sodium hydroxide; from about 0.5% to about 45% by weight amine or
ammonia; from about 0.25% to about 20% by weight lignin sulfonate and from
about 0-1% to about 10% by weight copper sulfate. Water may be used from 1%
to about 100% by weight.
Various formulations of this inYention were prepared and tested as
to their effectiveness for wood penetration and wood fixation properties.
This involved wood treatment, leaching tests and analysis. The leaching tests
and an~lysis generally conform to American Wood Preserver~s ~ssociation speci-
fications M11-66 Method to Determine Leachability of Wood Preservatives and
A5-76 Determination of Chloride f6r Calculating Pentachlorophenol in Solution
or Wood.
The experimental details of leachlng tests may bé described as
follows:
Four comparable 3/4" x 3/~ x 3/~" Douglas fir or Southern pine
sapwood blocks treated with like solution retentions were split in two groups.
The blocks in Group 1 were directly assayed for pentachlorophenol while the
-- 5 --


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Gro~p 2 blocks were leached and then assayed for pentachlorophenol. The blocks
were weighed before and after treatment to determine retentions. Retention
of control and leached blocks were considered and corrections made where
necessary. The percent pentachlorophenol retained in the leached blocks were
reported in the examples by use of the following equation:

leached blocks average PCP assay
_ x 100 = Percent preservative
retention in leached
unleached blocks average PCP assay blocks
The retained leaching water was also analyzed for preservative content. The
treating equipment used for the most part (small scale~ was that described in
the American ~ood Preserverr~s Association specification ~ 6, however, in

examples 12 and 13 a larger pilot plant operation was used. This is described
in the above noted examples.
In addition, treated wood speciment were given the soil block tests
according to AWPA Standard Method M10-63, using Madison 617, Lenzites Trabea
and Madison 698 Poria Monticola Murr fungi.
~`~ Fur~hermore, although it was originally intended that the treating
compositions of our invention were designed for landsite use, it was discovered
that the treated wood would withs~and a marine environment as shown in Examples
2 and 10. In these cases leaching with sea water was performed as well as
with tap water.

Also, solution stability tests were run to insure that they would
not form precipitates under normal treating conditions. Corrosion tests
confirmed that the systems are non-corrosive to steel. Bronze or copper should
not be used in treating plant equipment where these systems are involved.
h brief explanation of the design of the 42 experimental examples
follows:
Examples 1 through 13 demonstrate general formulations and testing
results of the invention. Examples 17 ~hrough 42 serve to demonstrate the


- wide latitude or ranges of formula ingredients and concentrations that are
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;3

suitable for obtaining acceptable wood treating solutions. Example 1~ serves
as a control for the above examples. The formulations in ~xa~ple 14 do not
incorporate the important alcohols of our invRntion and do not form good
solutions since formula solubility is absolutely essential for wood treating
purposes.
Although the examples here contain mostly 2% or 3~ pentachlorophenol,
they can be readily formulated to contain from 1% to 50% pentachlorophenol.
The 2% or 3% formulas are used because they more closely conform to the amount
generally used in commercially ~reated wood to me~t present military and

~nerican Wood Preservers Associations assay retention specifications.
These examples, in general, illustrate the facets and details of
this invention, but are not to be construed as limiting the scope to the same.
Example 1. - To make 2.5% (by weight) concentration of pentachlorophenol
(PCP) treating compositionL
FORMULA


2.5 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
8.0 lbs. ammonium hydroxide (28%~
83.5 Ibs. water
The ingredients can be mixed in any order in this and the following experiments,
but it is of convenience to dissolve the PCP in n-butyl alcohol (or other
alcohols) as solution number 1. Ammonium hydroxide is dissolved in the
water as solution number 2. Solutions numbers 1 and 2 are mixed together

to provide the final wood treating system. If formulations specify e~tra
ingredients, they can be added next.
The assay results on the borings after treatment of Douglas fir wood are as

follows:
Assay, Lbs.
Depth of Penetration ~S~ o~d


0.0~ to 0.5~ zone o.68
0.5" to 1.0" 7one 0.~1

9~ i3

AWPA leach test results: 79.5% preservative retained using control as 100%.
Example 2. - To make 2.0% (by weight) concentration of pentachlorophenol (PCP3
in treating composition.
FORMULA
2.0 lbs. pentachlorophenol
6.o lbs. n- buty] alcohol
8.o lbs. ammonium hydroxide (28%)
82.56 lbs. water
0.5 lbs. tetrasodium pyrophosphate
0.94 lbs. copper sulfate
The assay results on the borings after treatment of Douglas fir wood are as
~ollows:
Assay, Lbs.
Depth of Penetration ~ ~ 1
0.0~ to 0.5~ ~one 0.43
0.5~ to 1.0~l zone o.38
AWPA leach test results: 83.7% preservative retained using control as 100%.
AWPA leach test results (by use of sea water leach~nt): 80.0% preservative
lo retained using control as 100%.
Example 3. - To make 1.7% (by weight~ concentration pentachlorophenol (PCP3
treating composition.
F0 A
1.7 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
12.0 lbs. ammonium hydroxide (28%)
78.~ lbs. water
0.5 lbs. sodium dichromate
0.5 lbs. copper sulfate
0.5 lbs. tetrasodium pyrophosphate
The assay results on the borings after treatment of Douglas Fir wood are as
~ollows:
Assay, Lbs.
De~th of Penetration PCP,/cu. ft. wood
0.0" to 0.5~ zone 0.44
0.5" to 1.0" zone 0.30
AI~PA leach test results: 67.4% preservative retained using control as 100%.
Example 4. - To make 2.0% (by w~ght) concentration of pentachlorophenol (PCP)
8 '`

~3

in treating composition.
FORMULA
2.0 lbs. pentachlorophenol
6.o lbs. n-hutyl alcoho]
8.o lbs. ammonium hydroxide (28%)
82 . 5 lbs. water
0.5 lbs. sodium gluconate
l.0 lbs. copper sulfate
AWPA leach test results: 83.6% preservative retained using control as 100%.
Example_5. - To make a 2.0% (by weight) concentration of pentachlorophenol
(PCP) in treating composition.
FORMn1LA
2.0 lbs. pen-tachlorophenol (PCP)
6.o lbs. butyl alcohol
8.o lbs. ammoniu~l~hydroxide (28%~
82.7 lbs. water
0.3 lbs. sodium citrate
1.0 ]bs. copper sulfate
AWPA leach test results: 81.8% preservative retained using control as 100%.
xample 6. - To make 3.0% (by weight) concentration of pentachlorophenol (PCP~
in treating compos~tion.
FO~MULA
3.0 lbs. pentachlorophenol
6.o lbs. n-~utyl alcohol
8.o lbs. ammonium hydroxide (28%)
81.75 lbs. water
0.25 lbs. sodium N-dihydroxyethylglycinate
1.0 lbs. copper sulfate
AWPA leach test results: 98.5% preservative retained using control as 100%.
xam~le 7. - To make 2.0% ~by weight) concentration pentachlorophenol (PCP~
treating composition.
FO~MULA
2.0 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
8.o lbs. ammonium hydroxide (28%)
83.2 lbs. water
0.3 lbs. sodium N-dihydroxyethylglycinate
0.5 lbs. copper sulfate
AWPA leach test results: 80% preservative retained using control as 100%.
_ 9 _

853

Example 8. - To make 1.5% (by weight3 concentration pentachlorophenol (PCP3
in treating composition.
FORMULA
1.5 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
8.o lbs. ammonium hydroxide (28%)
83.5 lbs. water
0.5 lbs. sodium dichromate
0.5 Ibs. copper sul~ate
~WPA leach test results: 100% preservative retained using control as 100%.
Example 9~ - To make 2.0% (by welght~ concentration pentachlorophenol (PCP3
treating composition.
F~MULA
-
2.0 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
8.o lbs. ammonium hydroxide (28%~
83.o lbs. water
0.5 lbs. sodium dichromate
0.5 lbs. copper sulfate
AWPA leach test results: 100% preservative retained using control as 100%~
- Two treating compositions containing 2.0% (by weight~ concentra-
~ ~ .
tion of tetrachlorophenol (TCP) were made.
FORMULAE
a. 2.0 lbs. tetrachlorophenol
6.o lbs. butyl alcohol
8.o lbs. ammonium hydroxide (28%~
82.5 lbs. water
0.5 lbs. tetrasodium pyrophosphate
l.0 lbs. copper sulfate
AWPA leach test results: 91% preservative retained using control as 100%.
AWPA leach test results (by use of sea water leachant): 81.9% preservative
retained using control as 100%.
b. 2.0 lbs. tetrachlorophenol
6.o lbs. butyl alcohol
8.o lbs. ammonium hydroxide (28%~
82.5 lbs. water .
0.5 lbs. ammonium lignin sulfonate
l.0 lbs. copper sulfate
AWPA leach test results: 83% preservative retained using control as 100%.
.
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9~3

AWPA leach test results (by use of sea water leachant): 80% preservative
retained using control as 100%.
E~ample 11. - To make 2% (by weight) concentration of tetrachlorophenol (PCP~
treating composit~on.
FORMULA

2.0 lbs. tetrachlorophenol
6.o lbs. n-butyl alcohol
10.0 lbs. ammonium hydroxide (23%)
0.5 lbs. ammonium lignin sulfonate
1.0 lbs. copper sulfate
80.5 lbs. water
The assay results on the borings after treatment of the Douglas Fir wood are

as follows.
Assay, Ibs.
Depth of Penetration PCP/cu. ft. wood

0.0" to 0.5~ ~one 0.58
0.5~ to 1.0~ 7one o.66
Example 12. - To make 2.0% (by weigh~ concen~ration of pentachlorophenol


(~CP) in tre æing composition.
FORMULA

2.0 lbs. pentachlorophenol
0.5 lbs. sodium hydroxide
8-0 lbs. ammonium hydroxide(924%)
85.5 lbs. water
3.0 lbs. ammonium lignin sulfonate (51%~
1.0 lbs. copper sulfate
TEST CONDITIONS
The experiment using the above composition was conducted in a large scale
experimental retort 72 feet in length by 15 inches in diameter. The initial
vacuum was 28 inches Hg for one half hour, then 135 lbs. pressure was applied
to the treating load for 18 hours. The treated posts were 6 feet, 6 inches

long by 6-7 inches in diameter.
RESULTS ON SOUTHERN PINE POST TREATMENT
The assay results on the borings taken from the treated wood are as follows:

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8~3

A.ssay, lbs.
Depth of Penetration PCP/cu. _ft._ wood
.. . . _ _
0.0" to 0.5" zone 1.06
0.5" to 1.0" zone o.69
1.0" to 1.5" zone 0.69
1.5" to 2-0" zone 0.71
Example 13. - To make 2.0% (by weight) concentration of tetrachlorophenol
(TCP3 in treating composition.
FO~MULA

2.0 lbs. tetrachlorophenol
0.5 lbs. ~odium hydroxide
7.0 lbs. ammonium hydroxide (24%)
86.5 lbs. water
3.0 lbs. ammonium lignin sulfonate (51%)
1.0 lbs. copper sulfate
TEST CONDITIONS
The experiment using the above composition was conducted in a large scale
experimental retort 72 feet in length by 15 inches in diameter. The initial
vacuum was 28 inches Hg for one half hour, then 135 lbs. pressure was applied
to the treating load for 18 hours. The treated posts were 6 ft. 6 inches
long by 6-7 inches in diameter.
RESVLTS ON THE WOOD POST TREATMENT
. . ... _ . =
The assay resul~s on the borings taken from the treated Southern pine wood

are as follows:
Assay, lbs.
Depth of Penetration TCP~cu. ft. wood

0.0" to 0.5" zone 0-83
0.5" to 1.0" zone 0.57
1.0" to 1.5" zone 0.51
1.5" to 2.0" zone 0-47
The assay results on the borings taken from the treated Douglas fir wood are

as follows:
Assay, lbs.
Depth of P nctration TCPLcu. ft- wood

0.0~ to 0.5~ zone o.67
0.5" to 1.0" zone 0.40
Example 14. - To make 2 - 2.5 (by weight) concentration of pentachlorophenol~
in absence of n-butyl alcohol or other alcohols, the following formulas were
- 12 -

353

attempted:
FORMULAE

a. 2.0 lbs. pentachlorophenol
8.o lbs. ammonium hydroxide (~28%)
90.0 lbs. water

b. 2.5 lbs. pentachlorophenol
25.0 lbs. ammonium hydroxide (28%)
72.5 lbs. water

c. 2.5 lbs. pentachlorophenol
25.0 lbs. ammonium hydroxide (28%)
71.0 lbs. water
1.0 lbs. copper sulfate
0.5 lbs. tetrasodium pyrophosphate
These formulations formed insoluble mixtures and thus were no~ suitable for
wood treatments in the absence of butyl alcohol
Example 15. - To make 3.0% (by weight~ concentration of sodium pentachloro- -~
phenate in treating composition.
FORMULA

3.0 lbs. so~ium pentachlorophenate
; 4.0 lbs. n-butyl alcohol
93.0 lbs. water
The assay results on the borings after treatment of the Douglas Fir wood

are as follows:~
Assay~ lbs.
~,~ Dep _ of _enetra~ion PCP~cu. ft wood
lU
0.0" to 0.5" zone 0.90
0.5~ to 1.0~ zone 0-75

AI~PA leach test results: 20.8% preservative retained using control as 100%.

Example 16. - A 3.0% (by weight~ concentration of sodium pentachlorophenate


in treating composition was made in the absence of butyl alcohol.

FORMUEA
` -$.o 1~ s~dium pentachlorophenate
-- 97~0 lbs. water
The assay results on the borings after treatment of Douglas Fir wood are as
follows:


- 13 -

9~53

Ass~y, Ibs.
Depth of Pene~ration PCP/cu- ft. wodd
0.0" to 0.5" zone 1.1
0.5~ to 1.0~ zone 0-04
Example 17~ - To make 2.5% (by weight) concentration ofpentachlorophenol (PCP)
treating composition.
FO~MULA
2.5 lbs. pentachlorophenol
8.o lbs. n-propanol
8.o lbs. ammonium hydroxide ~28%)
81.5 lbs. water
Exam~le 18. - To make 2.5% (by weight~ concentration of pentachlorophenol
(PcP) in treating composition.
FORMULA
2.5 lbs. pentachlorophenol
10.0 lbs. allyl alcohol
8.0 lbs. ammonium hydroxide (28%)
79.5 lbs. water
Example 19. - To make 2.5% (by weight~ concentration of pentachlorophenol
(PCP3 in treating composition.
FO~MUI31,s.
2.5 lbs. pentachlorophenol
6.o lbs. secondary butyl alcohol
8.o lbs. ammonium hydroxide (28%)
83.5 lbs. water
Example 20. - To make 2.5% (by weight) concentration of pentachlorophenol
(PCP~ in treating composition.
ORMULA
2.5 lbs. pentachlorophenol
6.o lbs. iso-butyl alcohol
8-0 lbs. ammonium hydroxide (28%3
83.5 lbs. ~ater
Example_21. - To make 2.5% (by w~ight~ concentration of pentachlorophenol
(PCP) in treating composition.
FORMULA
2.5 -lbs. pentachlorophenol
10.0 lbs. tertiary butyl alcohol
_ ~ _

~ $853

8.o lbs. ammonium hydroxide (28%)
79.5 lbs. water
Exa~ 22. - To make 1.0% (by weight~ eoncentra~ion of pentachlorophenol
(PCP) in a treating composition.
1.0 lbs. pentachlorophenol
2.0 lbs. n-butyl alcohol
3.0 lbs. ammonium hydroxide (28%3
94.0 lbs. water
Example 23. - To make 0.1% (by weight) concentration of pentachlorophenol
(PCP) in a treating composition.
FO~MULA
0.1 lbs. pentachlorophenol
2.0 lbs. n-butyl alcohol
2.0 lbs. ammonium hydro~ide ~28%'~
95.9 lbso water
Example 24. - To make 10.0% (by weight3 coneentration of pentachlorophenol
~P
(PCP) in a treating composition.
FORMULA
10.0 lbs. pentachlorophenol
12.0 lbs. n-butyl alcohol
12.0 Ibs. ammonium hydroxide (28%3
66.o lbs. water
E_a_ple 25. - To make 1.0% (by weight) eoncentration of pentachlorophenol
(PGP3 in a treating eomposition.
FORMULA
1.0 lbs. pentaehlorophenol
97.0 lbs. n-butyl aleohol
2.0 lbs. ammonium hydroxide ~28%3
Example Z6. - To make 50.0% (by weight~ eoneentration of pentaehlorophenol
(PCP) in a treating eomposition.
FORMULA
50.0 lbs. pentaehlorophenol
48.o lbs. n-butyl aleohol
2.0 lbs. ammonium hydroxide (28%3
- To make 25.0% (by weight3 eoneentration oP pentaehlorophenol
(PCP~ in a treating composition.
- 15

8S3

FDRMULA
25.0 lbs. pentachlorophenol
30.0 lbs. n-butyl aLcohol
45.0 lbs. ammoniwm hydroxide (28%)
Ex m~le 28. - To make 2.0% (by weight) concentration of pentachlorophenol
(PCP) treating composition.
FORMULA
2.0 lbs. pentachlorophenol
6.o lbs. n-butyl aLcohol
8.o lbs. ammonium hydroxide (28%~
1.0 lbs. copper sulfate
lo.o lbs. sodiwm N-dihydroxyethylglycinate
73.0 lbs. water
E~ample 29 - To make 2.5% (by weight) concentration of pentachlorophenol
(PCP) treating composition.
FO~MULA
2.5 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
15.0 lbs. ammoniwn hydroxide (14%)
76.5 lbs. water
E~am~le 30. - To make 2.0% (by weight~ concentration of pentachlorophenol
(PCP) treating composition.
FORMULA

2.0 lbs. pentachlorophenol
4.0 lbs. n-butyl alcohol
4.0 lbs. isopropyl alcohol
80.5 lbs. water
8.o lbs. ammoniwn hydroxide (28%3
0.5 lbs. tetrasodiwn py~ophosphate
1.0 lbs. copper suLfate
E~ample 31. - To mak0 3.0% (by weight) concentration of pentachlorophenol
(PCP) treating composition.
FORMULA
- 3.0 :Lbs. pentachlorophenol
4.0 lbs. n-butyL alcohol
4.0 lbs. isopropyl alcohol
81.0 lbs. water
8.o lbs. ammoniwm hydroxide (28%~
E~am~le 32. - To make 2.0% (by weight~ concentration of pentachlorophenol
- 16 -

8S;3

(PCP) in a treating composition.
FORMULA
2.0 :Lbs. pentachlorophenol
4.0 lbs. n-butyl alcohol
4.0 lbs. isopropyl alcohol
80.5 lbs. water
8.o lbs. ammonium hydroxide ~28%)
0.5 lbs. tetrasodium pyrophosphate
1.0 lbs. copper sulfate
Example 33. - To make 2.0% (by weight) concent~ation of pentachlorophenol
(PCP~ in a treating composition.
FORMULA
2.0 lbs. pentachlorophenol
6.o lbs. butyl alcohol
3.0 lbs. triethyl amine
85.5 lbs. water
0.5 lbs. tetrasodium ~yrophosphate
3.0 lbs. acetone
E~ample 34. - To make 2.0% (by weight3 concentration of pentachlorophenol
(PCP) in a treating composition.
FO~MULA
2.0 lbs. pcntachlorophenol
6.o lbs. butyl alcoho~
3.0 lbs. trimethyl amine
89.o lbs. water
Example 35. - To make 2.0% (by weight~ concentration of pentachlorophenol

(PC~) in a treating composition.
FORMULA
2.0 lbs. pentachlorophenol
6.o lbs. butyl alcoh~l
3.0 lbs. methyldiethanolamine
89.o lbs. water
Example 36. - To make 2.0% (by weight~ concentration of pentachlorophenol
(PCP~ in a t~eating composition.
FORMULA
2.0 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
8900 lbs. water
300 lbs. methyl anine
- 17 -


~i3

Ex mple 37. - To make 2.0% (by weight~ concentr.ation of pentachlorophenol
(PCP) treating composition.
FO~MULA
2.0 lbs. pentachlorophenol
6.o lbs. n-butyl alcohol
8.o lbs. ammonium hydroxide (28%)
82.0 lbs. water
1.0 lbs. a~noni~n lignin .sulfonate
1.0 lbs. copper sul~ate
Examele 3.8. - To make 2.0% (by weight) concentration of tetrachlorophenol-
pentachlorophenol treating composition.
FORMULA
l.o lbs. pentachlorophenol
1.0 lbs. tetrachlorophenol
6.o lbs. n-butyl alcohol
8~o lbs. ammonium hydroxide [28%~
82.5 lbs. water
0.5 lbs. ammonium lignin ~ulfate
1.0 lbs. copper sulfate
Example 39. - To make 2.0% (by weight) concentration of pentachlorophenol
(PCP~ treating composition.
FORMULA
2.0 lbs. pentachlorophenol
6 . o lbs. n-butyl alcohol
8.0 lbs. ammonium hydroxide (28%~
82.0 lbs. water
1.0 lbs. sodium lignin sulfonate
1.0 lbs. copper sulfate
Example 40. - To make 2% ~by weight) concentration of sodium pentachlorophenate
treating solution using sodium pentachlorophenate.
FO~MULA
12.0 lbs. sodium pentachlorophenate (16.7% concent~ate~
74~0 lbs. water
10.0 lbs. ammoni~n hydroxide
3.0 lbs. ammonium lignin sulfonate
1.0 lbs. copper sulfate
Exam~le 41. - To make a 2% (by weight) concentration of sodium pentachloro-
phenate treating solution using pentachlorophenol.
FOR~nJLA
- 18 -



.: ., ,' - ' ' , . . , :

~g~S3
2.0 lbs. pen-tachlorophenol
0.75 lbs. sodium hydro~ide
83.25 lbs. water
10.0 lbs. ammonium hydroxide
3.0 lbs. ammonium lignin sulfonate
1.0 lbs. copper sulfate
Example 42. - To make a 2% (by weight) concentration of sodium tetrachloro-
phenate treating solution using tetrachlorophenol
2.0 lbs. tetrachlorophenol
o.6 lbs. sodium hydroxide
83.4 lbs. water
10.0 lbs. ammonium hydro~ide
3.0 lbs. ammonium lignin sulfonate
1.0 lbs. copper sulfate




19



,

Representative Drawing

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date 1981-04-28
(22) Filed 1978-04-17
(45) Issued 1981-04-28
Expired 1998-04-28

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1978-04-17
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
REICHHOLD CHEMICALS, INC.
Past Owners on Record
None
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Drawings 1994-03-15 1 15
Claims 1994-03-15 2 85
Abstract 1994-03-15 1 45
Cover Page 1994-03-15 1 20
Description 1994-03-15 21 792