DE1617970C - Highly concentrated pentachlorophenol preparation - Google Patents

Description

used purposes. So although the concentrate according to the invention is a mixture is made up of dissolved pentachlorophenol and its reaction products, the amount of pentachlorophenol calculated in the concentrate and reported as such.

The pentachlorophenol is to carry out the reactions described above first in one Part of an alcohol dissolved along with the hydroxide. Isopropyl alcohol is the preferred alcohol, However, other monohydric aliphatic alcohols containing 1 to 3 carbon atoms can also be used, be used as part or all of the base solvent. Such alcohols are methanol and ethanol mentioned. Ethanol is not as cheap as isopropanol because it is more expensive while methanol is is less desirable due to its greater toxicity. Potassium hydroxide is the preferred one Hydroxide, but other similar hydroxides, such as sodium hydroxide or Ammonium hydroxide.

The ethoxylated aliphatic amine is then dissolved in another part of the alcohol. This amine contains 1 to 2 nitrogen atoms and 8 to 22 carbon atoms in the aliphatic groups and 4 to 20 ethylene oxide adducts. The aliphatic groups of the compounds are preferably derived from common fats and oils, for example from those fats and oils that have aliphatic groups contain, which mainly have 8 to 18 carbon atoms.

The amine, having a nitrogen atom, has the general formula given below a temperature at least 5O ⁰ C to be heated. The desired reactions take place at room temperature. However, to ensure that the reactions are completed, it is beneficial to use some heat.

According to another procedure, the pentachlorophenol salt and the pentachlorophenol complex can be used formed separately and then together to obtain the final formulation be mixed.

The hydroxide reacts preferentially with the hydroxyl group of the pentachlorophenol rather than with the Alcohol group of the solvent. As a result, side reactions with the solvent normally occur not on. The pentachlorophenol salt, which is formed by the reaction with the hydroxide can be expressed by the following formula:

. (CH ₂ CH ₂ O) ₃ , H.

R-N

35

^v (CH ₂ CH ₂ O) J, H

wherein X is an alkali metal or ammonium.

The amine forms a complex with the pentachlorophenol and does not enter into any reactions or complex formations with the solvent. The complex can be generalized by the following Formula to be reproduced

Cl Cl

wherein R stands for an aliphatic group having 8 to 18 carbon atoms and χ and y are integers whose sum is 4 to 15. This known amine is referred to as amine I below.

The amine having 2 nitrogen atoms has the general formula given below

40 Cl-;

> - OH A

(CH ₂ CH ₈ O) * H

R - N CH ₂ CH ₂ CH ₂ N

(CH ₂ CH ₂ O) J, H

II

(CH ₂ CH ₂ O) ₂ H

wherein R stands for an aliphatic group having 8 to 18 carbon atoms and x, y and ζ are integers, the sum of which is 6 to 20. This particular amine is also known and is referred to below as amine II.

The part of the alcohol which contains the dissolved ethoxylated aliphatic amine is then mixed with the Mixed alcohol content, which contains the dissolved pentachlorophenol and the hydroxide. The united Mixing the two parts is then used to promote the formation of the pentachlorophenol salt as well as the pentachlorophenol complex heated. For this purpose, the mixture will be the most favorable heated under reflux conditions. Optionally, all of the ingredients can be stirred at room temperature mixed and with continuous stirring on

45

55

60

65 Cl Cl

wherein A is an ethoxylated aliphatic amine. After the reaction, all of the pentachlorophenol are in the form of the mixed reaction products of the hydroxide and the amine. It can however, some unreacted pentachlorophenol may also be present. All the effective ingredients will be on calculated on the basis of pentachlorophenol, then 0 to 30 percent by weight of the mixture of reaction products and pentachlorophenol in the form of free or unreacted pentachlorophenol, 30 to 70% is present as a hydroxide reaction product and 30 to 70% as an amine reaction product. The preferred one Mixture contains 5 to 20% pentachlorophenol along with 40 to 70% of the hydroxide reaction product and 40 to 70% of the amine reaction product.

example 1

A highly concentrated pentachlorophenol preparation is formulated as follows:

18.87 parts by weight of amine I (where the sum of χ + y = 5) is mixed with approximately 18 parts of isopropanol to form a solution. 40 parts by weight of pentachlorophenol are in 18.13 parts by weight of isopropanol together with 5 parts by weight of potassium

hydroxyd dissolved. The two solutions are then combined and under reflux conditions ! / Heated for 2 hours. The preparation obtained has after cooling to room temperature appears to be a clear solution and contains 40 percent by weight pentachlorophenol. She is easy in Water emulsifiable and readily soluble in oils such as petroleum fractions.

Example 2

According to the procedure described in Example 1, another formulation is prepared with the Exception that the components are combined in the following proportions:

Amine I.

Pentachlorophenol.

KOH

Isopropanol

The concentration obtained is opaque but does not contain any precipitates and is in Water emulsifiable and soluble in oils such as petroleum fractions.

Example 3

According to the procedure described in Example 1, another formulation is prepared with the Exception that the components are combined in the following proportions:

Amine I.

Pentachlorophenol.

KOH

Isopropanol

The concentrate obtained has the appearance of a clear solution and is easily emulsifiable in water and readily soluble in oils such as petroleum fractions.

Example 4

A further formulation is prepared according to the procedure described in Example 1, with the exception that amine I (in which the sum of x + y - 15) is used. The components are combined in the following proportions:

Amine I.

Pentachlorophenol.

KOH

Isopropanol

assume that the ingredients in the following proportions be united:

Amine I.

Pentachlorophenol.

KOH

Isopropanol

14.5

35.0

5.3

45.2

100.0

The concentrate obtained has the appearance of a ίο clear solution and is easily emulsifiable in water and readily soluble in oils such as petroleum fractions.

Example 6

According to the procedure described in Example 1, another formulation is prepared using amine I (x + y = 15), with the exception that the ingredients are combined in the following proportions:

Amine I 6.4

Pentachlorophenol 35.0

KOH 6.3

Isopropanol 52.3

'

The concentrate obtained is opaque, but does not show any precipitates. It's easy in water emulsifiable and readily soluble in oils such as petroleum fractions.

Example 7

According to the procedure described in Example 1

another formulation is prepared, with the exception that amine II (where the sum of χ + y + ζ = 20) is used. The components are combined in the following proportions:

106.0

The concentrate obtained contains 30.3 percent by weight of pentachlorophenol and has the appearance a clear solution. It is easily emulsifiable in water and in oils, such as petroleum fractions, easily soluble.

Example 5

According to the procedure described in Example 1, another formulation is prepared using amine I (x + y = 15), with the result

Amine II

Pentachlorophenol.

KOH

Isopropanol

6.5 35.0

4.0 60.5

106.0

The concentrate obtained contains 30.3 percent by weight of pentachlorophenol and has the appearance a clear solution. It is easily emulsifiable in water and in oils, such as petroleum fractions, easily soluble.

Example 8

According to the procedure described in Example 1, another formulation is prepared using amine II (x + y + ζ = 20), with the exception that the ingredients are combined in the following proportions:

Amine II 18.87

Pentachlorophenol 40.00

KOH 5.00

Isopropanol 36.13

100.00 The concentrate obtained has the appearance of a

clear solution and is easily emulsifiable in water and readily soluble in oils such as petroleum fractions.

Claims (6)

1 2 Pentachlorophenol is a patent claims on an industrial scale: chemical used, which is widely used as a contact herbicide, poison laid out on the ground 1.Highly concentrated pentachlorophenol additive and as a plant peeling agent is used, rcitung, characterized by a) a 5 pentachlorophenol is also used as a protective agent for Alcohol base solvent made from monovalent rigging, leather, textiles, wood, lumber products aliphatic alcohols with 1 to 3 carbon or the like. Used. However, pentachlorophenol lies atoms consists, b) the reaction product is in solid form and is in an oil or water pentachlorophenol with alkali hydroxides and vehicles only poorly soluble or emulsifiable. The bis-ammonium hydroxide existing inorganic io her usual practice, pentachlorophenol in any Hydroxides, c) to dissolve or emulsify the reaction product of penta vehicle, consisted of chlorophenol with an ethoxylated aliphatic the pentachlorophenol in a suitable inactive Amine containing 1 to 2 amine nitrogen atoms and 4 bis solvent formulation to form a conc-20 Ethylene oxide groups as well as 8 to 22 carbon trats to dissolve, which then · in water has atoms in the aliphatic group, and 15 can be emulsified or dissolved in an oil. d) Pentachlorophenol, with the concentrate up to The use of an oil or water vehicle 40% by weight of pentachlorophenol in the form depends on the purpose of the treatment. For example a mixture of the reaction products and penta, the compound is usually in the form of a contains chlorophenol and the mixture of 0 to aqueous emulsion for use as a contact herbicide 30% pentachlorophenol, 30 to 70% of the hydroxide 20 used, while it is used as an oil solution (for example reaction product and 30 to 70% of the amine reaction fuel oil or kerosene) as a wood preservative. tion product. is brought. 2. Concentrate according to claim 1, characterized so far contained the so-called »liquid conc. that the alcohol from isopropanol central «from pentachlorophenol, which is dissolved in oil consists. 25 and could be dispersed in water, in fact 3. Concentrate according to claim 1, characterized in relatively small amounts of pentachlorophenol. Over-marked, that the hydroxide consists of potassium-moderate amounts of pentachlorophenol separate hydroxide. . namely from and do not dissolve in the concentrate. 4. Concentrate according to claim 1, characterized in that this restriction has the effectiveness of such indicates that the aliphatic amine has reduced the formula 3 ° concentrates, since the amount of the in the (ΓΗ ΓM Oi H oil or water vehicle introduced pentachlorophenols . (. LM ₂ LH ₂ U) _x H j _{m opposite to} J ₀₁ . Amount of inactive solution R-N medium, which is used to dissolve the pentachlorophenol (CHoCH, O) H must be used in order for this chemical to be used in the ² " ^y 35 vehicle is soluble or emulsifiable, is relatively small. It has also been found that some penta-8 to 18 carbon atoms and χ and y are whole chlorophenol concentrates not for use in numbers, the sum of which is 4-15. Hard water vehicles are suitable as a part 5. Concentrate according to claim 1, characterized in that the pentachlorophenol precipitates, so that in this way indicates that the aliphatic amine formula 4 ° further reduces the effectiveness of the concentrate (CH CH O ^ H will. ^{2 2} It is therefore an object of the present invention R —N in creating an improved highly concentrated ^x (CHoCH ₂ O) J / H Pentachlorophenol preparation which is dissolved in a water 45 vehicle is emulsifiable and soluble in an oil vehicle where R is for an aliphatic group with and a higher concentration of pentachlorophenol 8 to 18 carbon atoms and χ and y have whole, than is the case with the previously known preparations Are numbers that sum 4 to 5. was the case. In particular, the 6. Concentrate according to claim 1, characterized according to the invention preparation for use in hard indicates that the aliphatic amine has the formula 5 ° water. i H It was found that a pentachlorophenol j ₁ η (CH, CHO) H concentrate can be produced, which contains up to 40 I / ' ^{2 contains 2 y} weight percent dissolved pentachlorophenol, if RN CH ₂ CH ₂ CH ₂ N ^ d _as pentachlorophenol in a first Alkoholgrund- (CH ₂ CH ₂ O) ₂ H 55 solvent and then with a inorganic hydroxide as well as with an ethoxylated one where R is reacted with an aliphatic amine for an aliphatic group. The result is 8 to 18 carbon atoms and x, y and ζ of these conversions are a mixture of integers, the sum of which is 6 to 20. inorganic salt of pentachlorophenol, which 60 is formed from the hydroxide, a complex between the pentachlorophenol and the amine and some unreacted pentachlorophenol. This Mixture is easily emulsifiable in water and soluble in oil without precipitating. Further The invention relates to a highly concentrated Penta- 65 has been found that the reaction products in Chlorophenol preparation, which in vehicles from hard functional point of the pentachlorophenol insofar or soft water or oil dispersed are equivalent, as they have the same effect as pure can. Exercise pentachlorophenol if they are for the specified