JPS59134704A - Production of evaporating insecticide - Google Patents

Abstract

PURPOSE:p-Dichlorobenzene is, when necessary, combined with a solid adsorbent, then compressed into solid base balls and the balls are impregnated with a volatile insecticide to produce a solid evaporating insecticide composition with industrial advantage. CONSTITUTION:p-Dichloobenzene, naphthalene, ethane hexachloride, camphor, borneol or their mixture is combined with a solid adsorbent and/or absorbing extender, when necessary, and the mixture is compressed into solid ball base (the first stage). Then, the resultant balls are impregnated with a volatile insecticide such as dimethyl 2,2-dichlorovinyl phosphate, dimethyl 2,2-dichloro-1,2-dibromoethyl phosphate or their mixture as such or in the form of a solution in an organic solvent (the second stage). These processes gives a solid evaporating insecticial composition at room temperature in a shorter time than in the conventional process with simpler installment.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a novel method for producing a solid insecticide composition that evaporates at room temperature.

More specifically, the present invention provides solid organic substances that are vaporizable (sublimable) at room temperature, such as p-dichlorobenzene, naphthalene, hexachloroethane, camphor tree, or dragon tree, or any mixture thereof. The first step is to blend an adsorbent and/or an absorbent bulking agent into a solid matrix mass by compression, and add dimethyl-2 as a volatile insecticide that is liquid at room temperature to the solid matrix mass obtained in this way. , 2-dichlorovinyl phosphate (DDVP) and (or) the desired amount of 1,2-dibrominated rA 6-form of DDVP, that is, dimethyl-2,2-dichloro-1,2-dibromoethyl phosphate, as is or The present invention relates to a method for producing a solid insecticide composition that transpires at room temperature, which is characterized by combining the second step of dissolving and impregnating it in an organic solvent.

Now, this type of solid insecticide composition itself is already known, for example, from Japanese Patent Publication No. 39-20737 and others.

However, as clearly shown in each example of the above-mentioned literature, such a known solid insecticide composition is completely different from the above-mentioned specific manufacturing method of the solid insecticide composition of the present invention. A volatile organic substance such as p-dichlorobenzene is first heated and melted at room temperature, a predetermined amount of a transpirable insecticide component such as DDVP is added and dissolved at room temperature, and this is cooled to form an insecticide composition of the same shape. (Example I, ■ and (4) of the above document, right column No. 21-
(See line 22).

The present inventors used p-dichlorobenzene as a substrate and developed DDV.
As a result of further attempts to produce a solid insecticide composition using a known melting method as described in the above-mentioned document, in which P is used as an insecticide component, it was observed that stiffness has the following drawbacks.

DD when melting +)-dichlorobenzene
During melting and mixing of VP and cooling, losses due to volatilization of both components are significant. Furthermore, since these two components have different volatilities, their initial blending ratio does not match the blending ratio of the completed solid composition.

Port 6: In order to maintain a sanitary working environment during the above operations, ventilation equipment must be perfected.

C. The finished solid composition is stored at room temperature and during use, p-
Since dichlorobenzene gradually crystallizes and separates, the component ratio of the composition becomes locally non-uniform, and therefore it is not possible to ensure the transpiration of the insecticide components in an even ratio.

Second, this melting method generally requires a long working time.

As a result of various studies conducted by the present inventors, it has been surprisingly observed that the drawbacks A, C, C, and II of the above-mentioned known methods can be completely eliminated by implementing the method of the present invention specified above. Indeed, the new method of the present invention has been completed.

In the second step, the solid matrix mass obtained by compression in the first step according to the method of the present invention is impregnated with the specified insecticide component (eg DDVP) by dropping, injecting or injecting the insecticide component at room temperature. This can be carried out very quickly by immersion suction, and the insecticide component impregnated in this way is evenly distributed throughout the interior of the solid matrix mass, for example a cylinder or cube.

Therefore, the method of the present invention is extremely advantageous in industrial production, since the working time is shorter than the known melt-cooling solidification method, the equipment for carrying out the method is extremely simple, and the finished product is homogeneous. Incidentally, unlike the method of the present invention, the powder of the above substrate material is, for example, liquid DDVP.
If the mixture is pre-mixed with a certain proportion of DDVP and is compressed to form a solid mass, there is a drawback that DDVP oozes out during the pressurizing operation, but such undesirable development does not occur in the implementation of the method of the present invention.

The degree of compaction in the first step of the process of the invention has some influence on the legal capacity of the pesticide component in the second step. That is, if the degree of compression is too high, the microdensity of the molded nodules becomes large, which tends to reduce the rate of distribution of the insecticide and the maximum legal amount of the insecticide. However, in carrying out the process of the present invention, the optimum degree of compaction to produce agglomerates of substrate components suitable for the desired insecticide content can be readily determined by preliminary experiments. Generally, this compressive force is 30-60 kg/cm' preferably 40-50 k1
Although the range is 9 Am2, the upper and lower limits are not limiting. If the specified amount of the insecticide component to be contained in a certain amount of substrate nodule obtained by such appropriate compression is very small, it may be added to an appropriate organic solvent to evenly impregnate the nodule. It is best to dissolve and increase the volume before use. On the other hand, if Taiwan wants to have a large amount of insecticide ingredients, an appropriate amount of activated carbon, activated alumina, silica gel, etc.
By appropriately incorporating an adsorbent or absorbent such as LM calcium, magnesium carbonate, magnesium oxide, diatomaceous earth, or montmolinite, the amount of pesticides in Taiwan can be increased. Furthermore, some phenols may be added to one or the other of the nodule matrix components as a decomposition inhibitor (stabilizer) for layer colorants, fragrances, and/or specific insecticide components. Therefore, it should be understood that all of the above-mentioned auxiliary operations belong to the inventive concept of the method of the present invention.

For the compression of the substrate material in the first step of the method of the present invention, any means such as a load, hammering, compressed air, water pressure, oil pressure, etc. can be employed. Furthermore, the legalization rate can be increased if the rimming operation of the insecticide component in the second step of the present invention is performed under reduced pressure. An additional advantage of operating under reduced pressure is that decomposition of the pesticide by atmospheric moisture is avoided.

Before explaining the present invention using Examples below, the following Comparative Examples were conducted for reference.

The following ingredients were mixed uniformly in a beaker, and a compressed mass was made using a tablet press and observed.

A, p-dichlorohenzea 959 and DDVP5 g, B
, p-dichlorobenzene 85g, naphthalene 109, D
DVP59, C0p-dichlorobenzene 94g, hexachloroethane 1g,
DDVP 5 g Structure of the tablet press used (a) Iron cylinder with inner diameter 5c+u and height 12 mm (thickness 8
mm), (b) A 1.5 cm thick iron disc-shaped anvil (Anobil) that fits into the bottom of the cylinder (a) and is removable.
, (C) a diameter 4. which slidably fits into the cylinder (a).
85, 1m in height, 16C7+1 iron cylinder, (a) iron cylinder C4 (weight ft 4.5kg) the above component blends A, B and C are separately filled into the cylinder of the tablet press;
The top of the iron cylinder (C) holding down the ingredient mixture inside the cylinder was struck at a final fall distance (head) of 46 cm, then the anvil at the bottom was removed, and the cylinder (C) was press-fitted to form the cylinder. The compressed mass was collected. Accordingly, the following values were observed for formulations A, B and C.

Height of filled compound without impact: 5.3 cm Height of compound after 1 impact: 4.2 cm 2 times p
II // :3.9cmG times
p p: 3,42cm 10 times
tt tt :3.2cm1
Compression ratio after 0 blows: 5.3: 3.2=1
: 0. In all cases of A, 'B, and O, after 10 blows, some DDVP oozed out onto the surface of the compressed mass. More specifically, the lower limit of the number of blows without oozing of DDVP from Formulation A was approximately 6 times (compression ratio 0,7), while the lower limit of the corresponding number of blows for Formulation B and C was lower than the lower limit of A. It also appeared to be somewhat lower.

Incidentally, a compression ratio of 1:0.5 to 1:0.7 is a preferable value in order to maintain the practical mechanical fastness of the finished nodules.

Therefore, the above comparative example was found to be unsuitable for industrial production due to the tendency of DDVP to leach out during the compression operation.

Example 1 In consideration of the results of the comparative example, only the components A', B' and C', which were obtained by removing the DDVP from the above component blends A, B and C, namely the substrate materials, were subjected to a similar final blow to a compression ratio of 1. : 0.6, 3.2 cm thick, 4.9 cm diameter nodules were made, and 5 g of DDVP (3.4 cc colored with a trace amount of red pigment) was dropped into each nodule and absorbed using a billet. , DDvP are both 25
Uniform permeation throughout the interior of the nodule was observed within seconds to 30 seconds. Even when the resulting insecticide-containing nodules were left indoors for 20 hours, no DDVP exuded or dripped from the nodules.

Example 2 In order to carry out the method of Example 1 under conditions favorable for mass production, a tablet press with a diameter of 7.0 cm iron cylinder and a 15 kg drop was used to make tablets with a diameter of about 7.0 cm by one blow. Country, height approx. 2.2 cm, weight approx. 100 g, compression ratio 1:0.6
It is now possible to obtain compressed nodules.

In this case, the necessary height of the Tsukuda was 56 sides. This head can be determined freely by changing the weight of the mallet. Add 34cc (approximately 5g) of DDVP to each of these compressed nodules.
When DDVP was dripped into the ring, permeation into the ring was rapid and uniform.

Example 3 Silica gel 209 was mixed with 100 parts each of the substrate materials A', B' and C' used in Examples 1 and 2, and a mass having a compression ratio of 0.6 was made according to Example 2, and DDV was applied to this mass.
10 g of P was added dropwise. In this case as well, DDVP was quickly legalized as in each of the above embodiments. Moreover, when this baby boom was left hanging indoors, no DDVP oozed out. The nodules obtained in Examples 2 and 3 were placed in an aluminum can, with only the surface exposed,
The evaporation of DDVP and volatile base material evaporated was calculated every 10 days using a weighing scale, and the composition of the remaining nodule was analyzed and determined, and the result was almost the same as the initial composition of the nodule.

Therefore, it was confirmed that these compressed lumps are useful as solid transpirable insecticides.

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Claims (1)

[Claims] p-dichlorobenzene, naphthalene, hexachlorinated ethane, camphorwood, dragonwood, or any mixture thereof, with a solid absorbent and/or absorbent filler added as desired. a first step of forming a solid matrix mass by compression, and adding dimethyl-2,2-dichlorovinyl phosphate, dimethyl-2,2-dichloro-1,2- to the solid matrix mass thus obtained as a volatile insecticide component; A method for producing a solid insecticide composition that evaporates at room temperature, which comprises a second step of impregnating dibromoethyl phosphate or a mixture thereof as it is or by dissolving it in an organic solvent.