JP3327572B2 - Slime control agent - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

FIELD OF THE INVENTION The present invention relates to a slime control agent for industrial water having an improved effect.

[0002]

2. Description of the Related Art In industrial water, for example, pulp mills and paper mills used in pulp preparation and papermaking processes, papermaking water and cooling water, slime is formed due to propagation of microorganisms such as bacteria, yeasts and filamentous fungi, and various obstacles are caused. It is known to cause Slime can be used during the papermaking process, such as the wall of the riffler, screen, inlet or chest wall,
Almost every part of the process that uses water, such as white water pits and recovered white water pipe inner walls, gradually increases its thickness and eventually peels off and mixes into the pulp slurry,
Blocking screens and pipes. In this case, small slime lump mixed in the pulp slurry causes yellow or brown spots on the paper, so-called eyeballs, deteriorating the paper quality, and large slime lumps cause the paper to run out.

In recent years, improvement in white water recovery rate, eutrophication with additives such as starch and polyacrylamide, sediments containing inorganic fillers, resin components of wood, pitch-like sediments due to adhesives derived from waste paper, etc. As a result, the papermaking process has become an environment more suitable for the propagation of microorganisms. In particular, an improvement in the recovery rate of white water facilitates the emergence of bacteria resistant to the slime control agent and the occurrence of a bacterial replacement phenomenon, which is a cause of a decrease in the efficacy of the control agent. For this reason, more slime control agents have been developed and used than before.

[0004]

However, at present, there is no slime control agent capable of maintaining sufficient efficacy under such conditions, and there is a demand for development of a satisfactory slime control agent.

[0005]

Means for Solving the Problems The present inventors have the general formula

Embedded image 5-chloro-2,4,6-trifluoroisophthalonitrile represented by the following formula:

Embedded image By using in combination with 1,1-dibromo-1-nitro-2-acetoxyethane represented by the formula, it was found that an excellent synergistic effect which could not be expected from the case where these compounds were used alone was obtained. Based on this, the present invention has been completed.

[0006] 5-chloro-2,4,6-trifluoroisophthalonitrile and 1,1-dibromo-1-nitro-2
-The mixing ratio with acetoxyethane is 5:95 to 9 by weight.
5: 5, preferably 10:90 to 90:10, especially 30: 7
0 to 70:30.

[0007] The slime controlling agent of the present invention is a compound of the formula (I)
It is preferable to use chloro-2,4,6-trifluoroisophthalonitrile and 1,1-dibromo-1-nitro-2-acetoxyethane dissolved in a solvent. In some cases, 5-chloro-2,4,6-trifluoroisophthalonitrile of the formula (I) may be used by dissolving in 1,1-dibromo-1-nitro-2-acetoxyethane. The concentration of the active ingredient is 1 to 95% (w / w), preferably 5 to 6
0% (w / w). In some cases, a suspending agent or an emulsifying agent may be used. The concentration of the active ingredient is 1-95%
(W / w) preferably 5 to 60% (w / w).

As the solvent, ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone and isophorone, benzene, toluene, xylene, 1,2-dimethyl-4-ethylbenzene, 1,3-dimethyl-4-ethylbenzene, 1,4-dimethyl -2-ethylbenzene,
1,2,3,5-tetramethylbenzene, 1,2,4
Aromatic hydrocarbons such as 5-tetramethylbenzene, glycol ethers such as ethylene glycol dimethyl ether and diethylene glycol dimethyl ether, ethylene glycol monoethyl ether acetate, diethylene glycol monoethyl ether acetate, 3-methoxybutyl acetate, and 2,2,4-trimethyl- 1,
Glycol ester ethers such as 3-pentadiol diisobutyrate and ethylene glycol diacetate;
Esters such as ethyl acetate, butyl acetate, dimethyl diethyl maleate, diethyl succinate and diethyl fumarate; carbonates such as ethylene carbonate and propylene carbonate; 1,2-dichloroethane;
1,1,1-trichloroethane, trichloroethylene,
Halogenated hydrocarbons such as chlorobenzene are used. These solvents may be used alone or in combination of two or more.

[0009] The preparation of the present invention may contain a surfactant. As the surfactant, a nonionic surfactant is preferable, and examples thereof include polyoxyethylene alkyl ether, polyoxyethylene oleyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene nonyl phenyl ether, and oxyethylene oxypropylene block polymer. The content of these surfactants is 0.1 to 30% (w / w), preferably 0.5 to 10% (w / w) based on the whole preparation.

The slime controlling agent of the present invention further includes a stabilizer, a bulking agent, and a stabilizer generally used in the production of a slime controlling agent.
Corrosion inhibitors, detergents, and other germicides can be added as appropriate. The amount of the slime control agent of the present invention added to the papermaking process varies depending on the water source, the paper, the addition method (continuous addition method, impact addition method), and the like. Is 0.5-50p
pm shows sufficient efficacy.

[0011]

EXAMPLES In the following formulation examples, parts mean parts by weight. Formulation Example 1 1,1-dibromo-1-nitro-2-acetoxyethane 10 parts 5-chloro-2,4,6-trifluoroisophthalonitrile 10 parts Propylene carbonate 80 parts were mixed to obtain a slime control agent. . Formulation Example 2 1,1-dibromo-1-nitro-2-acetoxyethane 20 parts 5-chloro-2,4,6-trifluoroisophthalonitrile 10 parts Propylene carbonate 70 parts were mixed to obtain a slime control agent. . Formulation Example 3 1,1-Dibromo-1-nitro-2-acetoxyethane 10 parts 5-Chloro-2,4,6-trifluoroisophthalonitrile 10 parts Dimethyl maleate 80 parts were mixed to obtain a frume controlling agent. Was.

Formulation Example 4 1,1-Dibromo-1-nitro-2-acetoxyethane 10 parts 5-Chloro-2,4,6-trifluoroisophthalonitrile 10 parts Propylene carbonate 40 parts 2,2,4-trimethyl 30 parts of 1,3-pentanediol isobutyrate 10 parts of polyoxyethylene oleyl ether (Emulgen 404, manufactured by Kao Corporation) were mixed to obtain a slime control agent. Formulation Example 5 1,1-dibromo-1-nitro-2-acetoxyethane 10 parts 5-chloro-2,4,6-trifluoroisophthalonitrile 10 parts Ethylene glycol diacetate 80 parts were mixed to give a slime control agent. Obtained.

Test Example 1 A. 70 ml of white water collected from each of the paper mills (a), (b) and (c) C. D liquid medium (20 ml) was added, and pre-culture was performed at 32 ° C. for 1.5 hours using a shaking incubator. This sample 4.5m
of the reagent was added to the culture cell, the reagent was added to a concentration of 30 ppm (the active ingredient was 6 ppm), and the mixture was shake-cultured at 32 ° C., and the addition of the drug was performed at the same time. The absorbance at 660 nm of these cultures was measured over time, and the absorbance value of 0.100, which had entered the growth phase, was regarded as the value of the start of growth. From the time required for the addition of the drug to reach 0.100, The time required for the drug-free sample (blank) to reach 0.1 is subtracted to obtain the growth inhibition time.

The growth inhibition times are shown in Tables 1 to 6 and compared. The growth inhibition time becomes longer as the effect of the reagent agent becomes stronger. These reagents were dissolved in 80 parts of propylene carbonate with the total of 1,1-dibromo-1-nitro-2-acetoxyethane and 5-chloro-2,4,6-trifluoroisophthalonitrile being 20 parts. At the time of addition, the mixture was diluted with diethylene glycol monoethyl ether acetate and used. The reagents in the table are as follows. A: 1,1-dibromo-1-nitro-2-acetoxyethane B: 5-chloro-2,4,6-trifluoroisophthalonitrile

[0015]

[Table 1]

[0016]

[Table 2]

[0017]

[Table 3]

Nos. 2 to 6 in Tables 1, 2 and 3 are slime controlling agents of the present invention, and others are comparative examples. From this, compared with the preparation containing the reagents A and B alone,
It is known to have better efficacy at the same active ingredient concentration.

Test Example 2 10 ml of white water collected from each of the paper mills (a), (b) and (c) was placed in an Erlenmeyer flask, and the reagent was supplied to the sample at 30 pp.
m (active ingredient 6 ppm) and added for 1 hour,
After contacting with the drug while shaking culture at 32 ° C., sampling was performed and the number of viable bacteria was measured. The bactericidal effect was known from the decrease in the number of viable bacteria in the sample, and was determined as the bactericidal power. The bactericidal efficacy was shown in Tables 4 to 6 and a comparative study was conducted. The higher the bactericidal activity of the reagent agent, the lower the viable cell count.

These reagents are prepared in the same manner as above.
A total of 20 parts of dibromo-1-nitro-2-acetoxyethane and 5-chloro-2,4,6-trifluoroisophthalonitrile was dissolved in 80 parts of propylene carbonate and diluted with diethylene glycol monoethyl ether acetate at the time of addition. Used. The reagents in the table are as follows. A: 1,1-dibromo-1-nitro-2-acetoxyethane B: 5-chloro-2,4,6-trifluoroisophthalonitrile

[0021]

[Table 4]

[0022]

[Table 5]

[0023]

[Table 6]

Nos. 2 to 6 in Tables 4, 5 and 6 are slime controlling agents of the present invention, and others are comparative examples. From this, it is known that, compared to a preparation containing the reagents A and B alone, the same active ingredient concentration has more excellent efficacy.

[0025]

The slime controlling agent of the present invention has an excellent slime controlling action over a long period of time, so that a small amount of slime controlling agent in industrial water can be prevented for a long period of time.

Continuation of the front page (72) Inventor Takuo Uejima 2-14-5 Hiranuma, Nishi-ku, Yokohama-shi, Kanagawa Pref. Permachem Asia Co., Ltd. 61402 (JP, A) JP-A-62-402 (JP, A) JP-A-3-167101 (JP, A) JP-A-4-9305 (JP, A) (58) Fields investigated (Int. ⁷ , DB name) A01N 37/34 104 A01N 37/48 C02F 1/50 532 CA (STN) REGISTRY (STN)

Claims (1)

(57) [Claims] 1. A compound of the general formula 5-chloro-2,4,6-trifluoroisophthalonitrile and 1,1-dibromo-1-nitro-2
95: 5 to 5: 9 with acetoxyethane as active ingredient
5. A slime control agent, which is contained at a ratio of 5.