DE1068943B - Process for the production of water-containing pastes based on ammonium salts of dinitrophenols for pest control - Google Patents

Description

Authority]

The dinitrophenols and their salts have been used for plant protection for many years. One uses they are used to treat fruit trees by atomizing the aqueous solution during dormancy,

It is also known to be the ammonium salt of dinitroocresol to be used as a herbicidal agent. But this compound is very sparingly soluble in water, especially when the farmer uses water at a temperature below 10 ° C, as is usually the case in winter Case is. It is then indispensable, the ammonium t ° Dinitrocresolate to be used in the form of extremely fine distribution.

The first dinitrophenols were sold as a dry, finely divided powder, but this had the disadvantage had that the dust irritated to sneeze and fell annoyingly due to a very strong coloring power.

Instead, slightly moistened powders were used, which are less irritating because they have less of a tendency to atomize when they are handled. The problem was so far not solved, ao as the damp particles tend during storage and transportation, "", "fr *" H "yyi ft to the Ammoniumdinitrokresolats | tifl |. Fen The production of broths daraas is not easy, and the Spray nozzles are often clogged, and the water tends to evaporate during storage, and yellow, irritating dust particles form on handling.

In order to get over these difficulties, the dinitrophenols are already available in aqueous form Suspensions sold. These pastes generally contain 40 to 60% of the active product in the condition very fine distribution, which considerably facilitates the preparation of broths. They are usually obtained by grinding the crystals of the ammonium dinitrocresolate in ball mills, hammer mills, stone mills etc. It is always necessary to convert the dinitricresol into the ammonium salt beforehand.

In general, the sodium salt of dinitrocresol is first prepared by hot soda allowed to act on molten dinitrocresol dispersed in a large amount of water, then one sets an ammonium salt, e.g. B. the ammonium sulfate, too. The ammonium dinitrocresolate then precipitates, and as soon as the contents of the vessel have reached the usual temperature, they are filtered and washed to remove what has formed Eliminate sodium sulfate, and then dry. The mother liquors contain a significant amount of ammonium dinitrocresolate, which must be recovered.

You can also work directly so that you ammonia at about 90 ° C with the molten and converts dinitrocresol dispersed in a large amount of water. It is also always necessary during the Filter and dry crystals formed after cooling.

Method of manufacture
of pastes containing water
based on ammonium salts of dinitrophenols for pest control

Applicant:

Societe Anonyme des Matieres Colorantes et Produits Chimiques de Saint Denis,

Paris

Representative:

Dr. phil. Dr. rer. pole. K. Köhler, patent attorney,
Mündien 2, Amalienstr. 15th

Andre Chomette, Neuüly-sur-Seine, Seine,

and Veuve Gabrielle Pechkranz,

St-Cloud, Seine-et-Oise (France),

have been named as inventors

These procedures require the use of a large one Expenditure of calories, as well as the use of large vessels, because you generally work at a lot great dilution.

The mixing of dinitro-o-cresol is also known, possibly in the moist state, with an alkali carbonate for the production of a spray for plant protection purposes.

According to the invention, however, is not an alkali carbonate, for. B. soda, but ammonia. The sodium salt of dinitro-o-cresol is lighter soluble in water as the ammonium salt, but in the dry It is explosive and irritates the mucous membranes. In addition, the sodium salt is used as a pesticide less effective.

The main reason why the ammonium salt has so far not been able to establish itself as a plant protection agent is line on the fact that it was previously not possible to bring it into a suitable form at low cost readily dissolves quickly in water, which is highly effective and convenient and harmless to the consumer handle is.

It has now been found that aqueous concentrated Suspensions of the ammonium salts of dinitrophenols in a microcrystalline state, their crystals are essentially smaller than 2μ, can be produced if one takes place directly in an aqueous medium without

9M6W394

Claims (1)

3 4 warm ammonia with the nitrated derivative of a borrowed point of view as unfavorable because it affects Phenol reacts, which is then necessary as a substituent, much more water for the same May contain alkyl groups and halogen atoms. Amount of active substance to be transported. It wasn't to be expected that you would get one in water like this. To ensure this cooling, one can Replace well as insoluble bodies with a concentrated 5 part of the water with ice. You can also use Dissolving ammonia without adding calories to the reaction mass converting the ammonia or the phenol can bring. add compound in portions, in such a way that the Surprisingly, the ammonium carbonate temperature remains below 25 ° C,
compared to dinitro-o-cresol significantly different from Na- You can use trium salts at the beginning or in the course of the preparation. It is known that a mixture of sodium carbonate and di-iodispersing and emulsifying agents, such as gum aranitro-o-cresol, does not form carbon, cellulose sulphite waste liquor or condensation products with water. Commercially available ammonium carbonate, on the other hand, by adding naphthalenesulfonic acids with formaldehyde, winds under the same circumstances and with little, if necessary, substances that keep the surface moisture in such a long-lasting foam that you reduce the tension. Anti-foaming agent, hygroscopic mixture in conventional atomizing devices do not add 15 pish substances, anti-gelling agents,
can handle. In order to separate the To avoid mixtures of finely ground dinitro-o-cresol and suspension, bentonite, carboxy- of finely ground ammonium carbonate and sodium methyl cellulose, salts of alginic acid, derivatives of poly- sulfate dissolve with water in the for agricultural acrylic acid, add polyvinyl alcohol, The use of suitable amounts is not nearly as ao The following examples explain the manner in which easily and completely how the present invention can be carried out according to the present invention, manufactured products. Most of the Dinitro- _Ώ . o-Jcresols remains undissolved. Example 1 The new process enables production to be maintained at a temperature below 25 ° C less explosive, even when drying out, and in as 200 kg dinitro-o-cresol, 68.8 kg 25 weight percent Water without clumping easily soluble pastes with ammonia and 151 kg of water or water with ice in a content of at least 50 ° / _0-di- ammonium in the presence of 12.5 kg successive Zellulosesulfitablauge nitro-o-cresolate. act. This new process is extremely economical, because 2 kg of carboxymethyl cellulose are added and a concentrated, aqueous suspension is obtained in small containers without fi l-30, which consists of microtrating, drying and washing concentrated water crystals of ammonium dinitro-o -cresolate. If necessary, the paste obtained from microcrystals of ammonium dinitro can be obtained by means of a pastes consisting of cresolate, which cannot be sent through to the mill,
together and dissolve quickly in water, also _R · -10
when the water temperature is close to 0 ° C. 35 ice cream ζ
These pastes, which have a content of about 40 to 60 percent of the active substance, sent through an attritor, can also be used to dilute the following mixture with a little water to obtain suspensions: 18, 5 kg of 25 weight percent ammonia, which are capable of atomizing directly onto the plants, 2.25 kg of gum arabic, 45 kg of crushed ice, 8.5 liters. 40 water and 65 kg dinitro-sec-butyl-phenol. In the case of Dinitrokresols is advantageous to use it in physi- containing the paste obtained at the outlet of the attritor Nigen condition which is easily obtained to 50 ° / ₀ ammonium salt of the dinitro-sec-butylphenol.
can, if you slowly stir an aqueous suspension of molten dinitrocresol with vigorous stirring.
cools down. 45 It may also be advantageous to use an aqueous suspension to prepare a concentrated process of Dinitro-o-cresol to be used. If necessary, water-containing paste, consisting of the ammonium they can be salted by grinding at ordinary temperature of a dinitrophenole, dinitroalkylphenol or in a ball mill or in another suitable one of a dinitroalkyl halophenol, especially des Mill received. 50 Dinitro-o-cresols, for pest control, thereby It is important that the mixture in the course of the characterized that the dinitrophenol with ammonia, Manufactured according to the heat generated to form an emulsifier and a little water mixed cool. Surprisingly, it has been found that or is triturated, with an over- this cooling is required to prevent suspensions from rising by 25 ° C. hold that when determining 50 or more ° / ₀ to 55 Give ammonium dinitro-o-cresolate. Considering the publications under consideration: Temperature can rise to 50 or 60 ° C, one can patent specifications No. 4000 and 4001 of the Office for only receive suspensions that are less rich in inventions and patents in Soviet Monium dinitro-o-cresolate are what differ from the economic statute zone of Germany. 909 648/394 11. »