CN110269066A - Compound disinfectant and its preparation method and application - Google Patents

Abstract

The invention discloses a kind of compound disinfectant and its preparation method and application, compound disinfectant is uniformly mixed by fluorine azoles bacterium acyl azanol, the ethylene glycol of 10~15 mass fractions and the softened water of 30~54 mass fractions of the dodecyl guanidine hydrochloride of 25~30 mass fractions, (E)-[2- [6- (2- cyano-benzene oxygen) pyrimidine-4-yl oxygen] phenyl] -3- methoxy-methyl acrylate of 5~10 mass fractions, the Didodecyl Dimethyl Dibenzyltinoammonium Chloride of 5~10 mass fractions, 1~5 mass fraction.Compound disinfectant of the invention is compounded non oxidizing bactericide, there is good synergistic effect, it endangers maximum three classes Pseudomonas to industrial circulating water: heterotrophism Pseudomonas, sulfate reduction Pseudomonas and Crenothrix have higher bactericidal effect, belong to environmentally friendly non oxidizing bactericide.

Description

Composite bactericide and its preparation method and application

technical field

The invention belongs to the technical field of water treatment agents for circulating cooling water systems, and in particular relates to a compound fungicide and its preparation method and application.

Background technique

A large number of microorganisms exceeding the standard cause the formation of rust and slime in the circulating cooling water system, which will lead to pipeline blockage and corrosion, and cause a series of negative effects on the continuous, stable and safe operation of the circulating water system. One of the big problems. The most common harmful microorganisms in circulating cooling water are heterotrophic bacteria, sulfate reducing bacteria and iron bacteria.

Water treatment bactericides refer to chemical substances that are highly sensitive to some microorganisms and can achieve antimicrobial properties when added in a small amount to water. They can control or kill microorganisms such as bacteria, algae and fungi in water. The use of various fungicides can quickly and efficiently kill harmful microorganisms in water. There are many types of fungicides. Some fungicides have a killing effect on a variety of microorganisms, while some fungicides only have a killing effect on a few types of microorganisms. The former are generally called "broad-spectrum" fungicides, while the latter are called "special purpose Sexual" fungicides.

At present, the commonly used fungicides in industrial circulating cooling water are geeramine, bromogeramine, isothiazolinone, etc. Although this type of fungicide has the characteristics of high efficiency, low toxicity, and not easily affected by pH changes, it has the disadvantages of large dosage, low bactericidal rate, or lack of broad-spectrum bactericidal effect when used alone.

Therefore, it is necessary to provide a compound fungicide and its preparation method and application to solve the above problems.

Contents of the invention

Aiming at the deficiencies in the prior art, the object of the present invention is to provide a preparation method of a compound fungicide.

Another object of the present invention is to provide the compound fungicide obtained by the above preparation method.

The purpose of the present invention is achieved through the following technical solutions.

A compound bactericide, which consists of 25-30 parts by mass of dodecylguanidine hydrochloride and 5-10 parts by mass of (E)-[2-[6-(2-cyanophenoxy)pyrimidine -4-yloxy]phenyl]-3-methoxymethyl acrylate, 5-10 parts by mass of didodecyldimethyldibenzyl tin ammonium chloride, 1-5 parts by mass of fluorine It is prepared by uniformly mixing pyraclostrobin, 10-15 parts by mass of ethylene glycol and 30-54 parts by mass of demineralized water.

The preparation method of the above-mentioned compound bactericide is carried out according to the following steps: the (E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methanol Mix the methyl oxyacrylate with the ethylene glycol evenly, add the demineralized water and stir evenly, then add the dodecylguanidine hydrochloride and stir evenly, and finally add the didodecanyldimethyldibenzyl Stir ammonium tin ammonium chloride and flufenapyramide evenly to obtain the composite fungicide.

The application of the above-mentioned composite fungicide in improving the sterilization rate of heterotrophic bacteria, sulfate-reducing bacteria and iron bacteria in water.

In the above technical solution, the bactericidal rate of the heterotrophic bacteria is 97-99.91%.

In the above technical solution, the bactericidal rate of the sulfate-reducing bacteria is 97-99.91%.

In the above technical solution, the bactericidal rate of the iron bacteria is 97-99.91%.

The invention mainly starts from the aspect of sterilization, not only achieves a good sterilization effect, but also has a higher sterilization rate for the common bacteria in the circulating cooling water, and keeps the number of microorganisms in the circulating cooling water system at a low level. Compared with the prior art, the present invention has the following significant advantages: (1) The three types of fungi that are most harmful to industrial circulating water: heterotrophs, sulfate-reducing bacteria and iron bacteria all have higher bactericidal effects. (2) The composite bactericide of the present invention is a composite non-oxidizing bactericide, which has a good synergistic effect. (3) Efficient, broad-spectrum, easy to degrade, no residue, belongs to environment-friendly non-oxidizing fungicide.

Detailed ways

Dodecylguanidine hydrochloride has the functions of stripping microbial film and sterilizing, has the characteristics of light resistance, heat resistance, pressure resistance, and stable properties, and belongs to the permeable bactericidal material that destroys bacterial cell walls and cell membranes; (E) -[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxymethyl acrylate is a novel, efficient, broad-spectrum, systemic, low toxicity , easy to degrade, no residue environment-friendly fungicide; didodecyl dimethyl dibenzyl tin ammonium chloride can effectively treat sulfate reducing bacteria, saprophytic bacteria and iron bacteria in circulating cooling water; Hydroxylamine has broad-spectrum, high-efficiency characteristics, which can enhance the synergistic effect of other fungicides.

The technical solutions of the present invention will be further described below in conjunction with specific embodiments.

The source or source of purchase of the drug is as follows:

(E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxymethyl acrylate was synthesized by the inventor, and the synthesis method can be found in the reference: Yi Min.Study on the synthesis process of (E)-2-{2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl}-3-methoxymethyl acrylate[J].Fine Chemical Raw Materials and Intermediates, 2012(12):11-20+5.

Dodecylguanidine hydrochloride was synthesized by the inventor. For the synthesis method, see references: Song Yongbo, Li Qiuxiao, Li Yunling, Zhi Lifei. Synthesis and properties of dodecylguanidine hydrochloride[J]. Fine Chemical Industry, 2013,30(01):28-31.

Flufenapyramide was purchased from Syngenta.

Example 1

The preparation method of compound bactericide, carries out according to the following steps: [with 10g (E)-[2-[6-(2-cyanophenoxy) pyrimidin-4-yl oxygen] phenyl]-3-methoxy Add 20g of ethylene glycol to methyl acrylate to dissolve, then add 108g of demineralized water and stir evenly, then add 50g of dodecylguanidine hydrochloride and stir evenly, and finally add 10g of didodecyldimethyldibenzyl chloride Ammonium stannate and 2 g of flufenapyramide were stirred evenly to obtain a compound fungicide.

Example 2

[The preparation method of compound bactericide, carry out according to the following steps: 11g (E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxy Add 21g of ethylene glycol to methyl acrylate to dissolve, then add 102g of demineralized water and stir evenly, then add 51g of dodecylguanidine hydrochloride and stir evenly, and finally add 11g of didodecyldimethyldibenzyl chloride Ammonium stannate and 4 g of flufenapyramide were stirred evenly to obtain a compound fungicide.

Example 3

The preparation method of compound bactericide, carries out according to the following steps: 12g (E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxy Add 22g of ethylene glycol to dissolve methyl acrylate, then add 98g of demineralized water and stir evenly, then add 52g of dodecylguanidine hydrochloride and stir evenly, and finally add 12g of didodecyldimethyldibenzyl chloride Stir ammonium tin and 4 g flufenapyramide evenly to obtain a compound fungicide.

Example 4

The preparation method of compound bactericide, carries out according to the following steps: 14g (E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxy Add 24g of ethylene glycol to dissolve methyl acrylate, then add 88g of demineralized water and stir evenly, then add 54g of dodecylguanidine hydrochloride and stir evenly, and finally add 14g of didodecyldimethyldibenzyl chloride Tin ammonium and 6 g of flufenapyramide were stirred evenly to obtain a compound fungicide.

Example 5

The preparation method of compound bactericide, carries out according to the following steps: 16g (E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxy Add 26g of ethylene glycol to dissolve methyl acrylate, then add 78g of demineralized water and stir evenly, then add 56g of dodecylguanidine hydrochloride and stir evenly, and finally add 16g of didodecyldimethyldibenzyl chloride Tin ammonium and 8 g of flufenapyramide were stirred evenly to obtain a compound fungicide.

Example 6

The preparation method of compound bactericide, carries out according to the following steps: 20g (E)-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxy Add 30g of ethylene glycol to dissolve methyl acrylate, then add 60g of demineralized water and stir evenly, then add 60g of dodecylguanidine hydrochloride and stir evenly, and finally add 20g of didodecyldimethyldibenzyl chloride Stir ammonium tin and 10 g of flufenapyramide evenly to obtain a compound fungicide.

In order to illustrate the bactericidal effect of the present invention, the performance of the compound bactericide prepared by the above-mentioned implementation is tested below. The water collected from the sewage treatment plant of Tianjin Vocational University was used as the inoculation. According to the following test method, the bacteria inoculated in the sewage treatment plant of Tianjin Vocational University were cultivated to obtain the water source to be tested, and the water source to be tested was tested according to the following test method. The test results are shown in Table 1.

Test method: The performance evaluation method of heterotrophic bacteria of compound fungicide adopts the test bottle method of extinction dilution method, and the performance evaluation method of sulfate-reducing bacteria adopts GB/T14643.5-1993 "Sulfate-reducing bacteria in industrial circulating cooling water MPN method for the determination of iron bacteria, the performance evaluation method of iron bacteria adopts GB/T14643.6-1993 "MPN method for the determination of iron bacteria in industrial circulating cooling water".

Table 1

Initial bacterial concentration: the concentration of bacteria in the water source to be tested.

Addition amount of compound fungicide: the mass of compound fungicide added per liter of water source to be tested.

It can be judged by the above data that the compound bactericide in the embodiment has a very good bactericidal effect on heterotrophic bacteria, sulfate reducing bacteria and iron bacteria in the water source to be tested, thus it can be seen that the compound bactericide can also have a positive effect on circulating cooling water. Very good bactericidal effect.

In order to illustrate the biodegradability of the composite bactericide of the present invention, the biodegradability of the composite bactericide prepared by the above-mentioned implementation is tested below (Guo Yong, Wang Hefang, Liu Zhiyong. Scale and corrosion inhibition properties of tobacco wood stalk extract [J] .Chemical Journal, 2014,65(01):298-304.), the biodegradability assay results are shown in Table 2.

Dissolve 50g of garden soil in 500mL of tap water, stir well and let stand for 2 hours, filter with coarse filter paper, use 200mL of filtrate as inoculum, mix 2mL of inoculum with 500mL of compound fungicide to obtain the solution to be tested, seal, Place it at a constant temperature of 25°C for 20 days, and measure the COD value of the test solution on the 20th day with reference to the potassium permanganate method (GB/T15456-2008).

Calculation of biodegradation rate:

Blank solution: prepare 200mL inoculum as a blank solution.

Degradation rate=[1-(Wt-W _t0 )/(W ₀ -W ₀₀ )]*100%.

W _t is the COD value that records the solution to be tested on the 20th day;

W _t0 is the COD value of the blank solution measured on the 20th day;

W ₀ is the initial COD value of the solution to be tested (initial: the 0th moment);

W ₀₀ is the initial COD value of the blank solution.

Table 2

It can be seen from Table 2 that the 20-day biodegradation rate is greater than 60%, which belongs to the easily degradable product and has relatively good biodegradability.

The present invention has been described as an example above, and it should be noted that, without departing from the core of the present invention, any simple deformation, modification or other equivalent replacements that can be made by those skilled in the art without creative labor all fall within the scope of this invention. protection scope of the invention.

Claims (6)

1. a kind of compound disinfectant, which is characterized in that by the dodecyl guanidine hydrochloride of 25~30 mass fractions, 5~10 mass (E)-[2- [6- (2- cyano-benzene oxygen) pyrimidine-4-yl oxygen] phenyl] -3- methoxy-methyl acrylate, 5~10 mass of number The Didodecyl Dimethyl Dibenzyltinoammonium Chloride of number, the fluorine azoles bacterium acyl azanol of 1~5 mass fraction, 10~15 mass parts The softened water of several ethylene glycol and 30~54 mass fractions is uniformly mixed.

2. the preparation method of compound disinfectant as described in claim 1, which is characterized in that carry out as steps described below: will be described (E)-[2- [6- (2- cyano-benzene oxygen) pyrimidine-4-yl oxygen] phenyl] -3- methoxy-methyl acrylate and the ethylene glycol are uniform Mixing, is added the softened water and stirs evenly, add the dodecyl guanidine hydrochloride and stir evenly, and is eventually adding double 12 Alkyl dimethyl dibenzyl ammonium stannic chloride and fluorine azoles bacterium acyl azanol, stir evenly, obtain the compound disinfectant.

3. the compound disinfectant that preparation method described in compound disinfectant as described in claim 1 or claim 2 obtains is improving Application in water in heterotrophism Pseudomonas, sulfate reduction Pseudomonas and Crenothrix sterilizing rate.

4. application according to claim 3, which is characterized in that the sterilizing rate of the heterotrophism Pseudomonas is 97~99.91%.

5. application according to claim 4, which is characterized in that the sterilizing rate of the sulfate reduction Pseudomonas be 97~ 99.91%.

6. application according to claim 5, which is characterized in that the sterilizing rate of the Crenothrix is 97~99.91%.