CN103734184A - Multiple-effect sterilizing agent and preparation method thereof - Google Patents
Multiple-effect sterilizing agent and preparation method thereof Download PDFInfo
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- CN103734184A CN103734184A CN201310660624.1A CN201310660624A CN103734184A CN 103734184 A CN103734184 A CN 103734184A CN 201310660624 A CN201310660624 A CN 201310660624A CN 103734184 A CN103734184 A CN 103734184A
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Abstract
The invention provides a multiple-effect sterilizing agent and a preparation method thereof, and raw materials comprise 30-40 parts of tert butyl alcohol, 15-30 parts of hydrogen peroxide, 5-15 parts of tungstic acid, 5-10 parts of cyclopentanecarboxylic acid, 10-20 parts of 5-chloro-2-methyl-4-isothiazoline-3-ketone, 2-8 parts of hydrochloric acid and 20-35 parts of water; the preparation method is as follows: putting a reaction kettle equipped with a condensation tube reactor in 35DEG C constant temperature environment, adding the tungstic acid into the reaction kettle, then adding the water, stirring for 10min under 65rpm conditions, evenly mixing, adding the hydrogen peroxide, stirring for 15-30min, then adding the tert butyl alcohol and the cyclopentanecarboxylic acid, continuing stirring for 20-40min, then adding a sterilizing agent, fully stirring for 15-40min, adding the hydrochloric acid, and stirring uniformly to obtain the multiple-effect sterilizing agent.
Description
Technical field
The present invention relates to the disposal of recirculated cooling water and oil field reinjection water, the product obtaining has efficiently, the feature of low toxicity,, good stability little to metal protection.
Background technology
Industrial circulating cooling water system provides essential nutrients and ion to microbial growth, in production process, the leakage of material is also for circulation microbial population provides nutriment, the exhibiting high surface providing by pipeline, heat exchanger, cooling tower filler and distributing pipe line system is long-pending, effectively promoted the growth of microbial population, microorganism grows to circulation and brings very big harm.The suspension of algae and sediments provide food for bacterium and mould, and the agglomerate that algae forms can stop up the pipeline in heat exchanger, reduces the flow of cooling water, thereby reduces the cooling effect of cooling water, reduces water quench effect, increases operating cost.Conventional broad-spectrum sterilization has nearly 40 years of the service time of isothiazolinone, dodecyl benzyl dimethyl ammonium chloride (1227) at present, exist drawback, the improper meeting of pH value accelerated corrosion system, is used this medicament for a long time, the pesticide resistance of bacterium is increased, and bactericidal effect reduces.
Literature search discloses: 1) Yang Yong; Bao Guozhu; Sun Zhikui; ; The research [J] of industrial circulating cooling water reuse; Water conservancy science and technology is with economical; 08 phase in 2007; 2) summer jewel, Ma Jiaxiang; Sulfate reducing bacteria is to corrosion of metal effect and control [J] thereof; Corrosion and protection; 04 phase in 1996; 3) Zhang Jianhua; " application Development Status and the development trend of cooling water treatment agent " [J]; Soda industry; 04 phase in 2003; 4) " recirculating cooling water system control of microorganisms " Sichuan Province Treatment of Industrial Water Engineering Technical Research Centre; 5) " harm of microorganism in cycle water " Zepu, Xinjiang petrochemical industry.
The new and effective Biocidal algae-killing agent of the present invention's development, both overcome the drawback of traditional bactericide, there is again efficient, low toxicity, little to metal protection, be subject to that organic substance influence is little, good stability, put prospect for sales on market good, checking after testing, the water quality that this product treatment is crossed meets the standard of GB-50050-2007 < < Code for design of industrial recirculating cooling water treatment > >.
Summary of the invention
The object of the invention is to: the multi-effect bactericide of development, effectively killing microorganisms, has that excitant is little, corrosivity is low, safety and low toxicity, is subject to the organic little technique effect that affects, for enterprise energy-saving and cost-reducing made demonstration.
The object of the present invention is achieved like this: a kind of multi-effect bactericide and preparation method thereof, with parts by weight preparation raw material and implement step by step;
Raw material: formed by tert-butyl alcohol 30-40 part, hydrogen peroxide 15-30 part, wolframic acid 5-15 part, ring valeric acid 5-10 part, CMIT 10-20 part, hydrochloric acid 2-8 part, water 20-35 part;
Preparation method: the reactor that condenser pipe is housed is placed in to the isoperibol of 35 ℃, first adds wolframic acid to reactor, then add water, under the condition of 65rpm, stir 10min, mix and add hydrogen peroxide, stir 15-30min, after mixing, add the tert-butyl alcohol and ring valeric acid, continue to stir 20-40min, then add bactericide, fully stir after 15-40min, continue to add hydrochloric acid to stir, obtain finished product.
Technical characterstic of the present invention and effect: to synthesize master, composite is auxiliary way, through the product that obtains of experiment, have good water-solublely, and little to metal system corrosion, its sterilizing rate reaches more than 99.5%; Product detects outward appearance and becomes light yellow transparent liquid; PH value (stoste) is 2.0-3.0; Density (20 ℃, g/cm
3) 1.0-1.08; Water-soluble: solvable, splendid for water treatment effect, realized former design object, show technological progress.
Embodiment
Below in conjunction with example, be further described.
Embodiment 1
Get 35 parts of tert-butyl alcohols, 20 parts of hydrogen peroxide, 5 parts of wolframic acids, 5 parts of ring valeric acids, 12 parts of CMITs, 3 parts of hydrochloric acid, 20 parts of water;
Preparation: the reactor that condenser pipe is housed is placed in to the isoperibol of 35 ℃, adds wolframic acid to reactor, then add water, under the condition of 65rpm, stir 10min, mix, add hydrogen peroxide, stir 15min, mix, add the tert-butyl alcohol and ring valeric acid, continue to stir 20min, then add bactericide, fully stir 15min, continue to add hydrochloric acid to stir, obtain multi-effect bactericide product.
Embodiment 2
Get 30 parts of tert-butyl alcohols, 15 parts of hydrogen peroxide, 5 parts of wolframic acids, 5 parts of ring valeric acids, 10 parts of CMITs, 2 parts of hydrochloric acid, 20 parts of water;
Preparation: the reactor that condenser pipe is housed is placed in to the isoperibol of 35 ℃, adds wolframic acid to reactor, then add water, under the condition of 65rpm, stir 10min, mix, add hydrogen peroxide, stir 30min, mix, add the tert-butyl alcohol and ring valeric acid, continue to stir 40min, then add bactericide, fully stir 40min, continue to add hydrochloric acid to stir, obtain multi-effect bactericide product.
Embodiment 3
Get 40 parts of tert-butyl alcohols, 30 parts of hydrogen peroxide, 15 parts of wolframic acids, 10 parts of ring valeric acids, 20 parts of CMITs, 8 parts of hydrochloric acid, 35 parts of water;
Preparation: in the reactor that condenser pipe is housed is positioned over the isoperibol of 35 ℃, add wolframic acid to reactor, then add water, under the condition of 65rpm, stir 10min, mix, add hydrogen peroxide to stir 20min, mix, add the tert-butyl alcohol and ring valeric acid, continue to stir 30min, add CMIT, fully stir 30min, add hydrochloric acid, multi-effect bactericide product stirs to obtain.
Multi-effect bactericide of the present invention, learns that physical and chemical index is: outward appearance: light yellow transparent liquid after testing; PH value (stoste): 2.0-3.0; Density (20 ℃, g/cm3): 1.0-1.08; Water-soluble: solvable.
This product and dodecyl benzyl dimethyl ammonium chloride (1227), isothiazolinone are carried out performance comparison evaluation for recirculated cooling water and oil field reinjection water and different microorganisms.
One, different quality Evaluation of Germicidal Efficacy
(1) Evaluation of Germicidal Efficacy in recirculated cooling water
Get 3 glasss of recirculated cooling waters that 100mL is identical, add respectively the following three kinds of medicaments of 25ppm, detect its bactericidal effect after placing the different time, the results are shown in Table 1.
Evaluation of Germicidal Efficacy in table 1 recirculated cooling water
From upper table data, learn, add the bactericide of equal number in recirculated cooling water, multi-effect bactericide is all higher than isothiazolinone, 1227 sterilizing rates, and sterilizing time keeps for a long time.
(2) Evaluation of Germicidal Efficacy in oil field reinjection water
Get 3 glasss of oil field reinjection waters that 100mL is identical, add respectively the following three kinds of medicaments of 50ppm, detect its bactericidal effect after placing the different time, the results are shown in Table 2.
Evaluation of Germicidal Efficacy in table 2 oil field reinjection water
From upper table data, learn, add the bactericide of equal number in oil field reinjection water, multi-effect bactericide is higher than isothiazolinone, 1227 sterilizing rates, and sterilizing time keeps for a long time.
Two, different bacterium Evaluation of Germicidal Efficacy
(1) to sulfate reducing bacteria Evaluation of Germicidal Efficacy
Get 3 glasss of identical water samples of 100mL, add respectively the following three kinds of medicaments of 30ppm, place after the different time, detect the bactericidal effect to sulfate reducing bacteria, the results are shown in Table 3.
The bactericidal property evaluation of table 3 to sulfate reducing bacteria
From upper table data, learn, add the bactericide of equal number in identical water sample, multi-effect bactericide is higher than isothiazolinone, 1227 stabilized efficiency, and sterilizing time keeps for a long time.
(2) to iron bacteria Evaluation of Germicidal Efficacy
Get 3 glasss of identical water samples of 100mL, add respectively the following three kinds of medicaments of 30ppm, place after the different time, detect the bactericidal effect to iron bacteria, the results are shown in Table 4.
The bactericidal property evaluation of table 4 to iron bacteria
From upper table data, learn, add the bactericide of equal number in identical water sample, it is high that multi-effect bactericide is killed iron bacteria efficiency than isothiazolinone, 1227, and sterilizing time keeps for a long time.
Three, the checking of multi-effect bactericide in production practices
The main bacteria that affects water quality in oil-field flooding is that sulfate reducing bacteria (SRB), saprophytic bacteria (TGB) and iron bacteria are because their growth conditions and metabolite thereof are different, on the impact of water filling also difference.They all belong to adheres to bacterium, very serious on the impact of flood pattern, and injection water quality is degenerated, and causes filling pipe and the perforation of pit shaft tube corrosion, stops up, even fracture.
(1) for the result of use of Xinjiang oil-contaminated water of oil field multi-effect bactericide, in Table 5.
Table 5 does not add the water quality table of multi-effect bactericide
| Sequence number | Analysis project | Unit | Analysis result |
| 1 | SRB | mg/L | ＞10 5 |
| 2 | TGB | mg/L | ＞10 5 |
Table 6 adds the water quality table of multi-effect bactericide
| Sequence number | Analysis project | Unit | Analysis result |
| 1 | SRB | mg/L | 1000 |
| 2 | TGB | mg/L | 100 |
(2) for the screening of Xinjiang oil-contaminated water of oil field multi-effect bactericide dosage: get 4 glasss of oil field reinjection waters that 100mL is identical, add respectively the multi-effect bactericide of 10ppm, 20ppm, 25ppm, 30ppm, after after placement 10min, detect its bactericidal effect, the results are shown in Table 6.
Table 6 adds the bactericidal effect of multi-effect bactericide
From upper table data, learn, in identical water sample, add the multi-effect bactericide of varying number, add 25ppm kill bacteria efficiency and want high.
The tert-butyl alcohol that this method is selected is by Yixing, Shanghai Run Jin Chemical Co., Ltd., hydrogen peroxide is provided by Urumchi exact science Instrument Ltd., wolframic acid is provided by Sheng Tianhengchuan bio tech ltd, Hubei, ring valeric acid is provided by Sheng Tianhengchuan bio tech ltd, Hubei, and CMIT Urumchi exact science Instrument Ltd. provides.
Claims (2)
1. multi-effect bactericide and preparation method thereof, is characterized in that: with parts by weight preparation raw material, implement step by step;
Raw material: formed by 20-35 parts, 30-40 parts of the tert-butyl alcohols, 15-30 parts, hydrogen peroxide, 5-15 parts of wolframic acids, 5-10 parts of valeric acids of ring, 10-20 parts of CMITs, 2-8 parts of hydrochloric acid, water;
Preparation: the reactor that condenser pipe is housed is placed in to the isoperibol of 35 ℃, adds wolframic acid to reactor, then add water, under the condition of 65rpm, stir 10min, add hydrogen peroxide, then stir 15-30min, add successively the tert-butyl alcohol and ring valeric acid, continue to stir after 20-40min, add bactericide, fully stir 15-40min, add hydrochloric acid, finished product stirs to obtain.
2. it is characterized in that in accordance with the method for claim 1: the raw material of selecting is commercially available prod.
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| CN201310660624.1A CN103734184A (en) | 2013-12-09 | 2013-12-09 | Multiple-effect sterilizing agent and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5785867A (en) * | 1993-08-05 | 1998-07-28 | Nalco Chemical Company | Method and composition for inhibiting growth of microorganisms including peracetic acid and a non-oxidizing biocide |
| US20100078393A1 (en) * | 2008-10-01 | 2010-04-01 | Bei Yin | Biocidal compositions and methods of use |
| CN102783482A (en) * | 2011-05-19 | 2012-11-21 | 大连百傲化学有限公司 | 3-isothiazolinone composition |
-
2013
- 2013-12-09 CN CN201310660624.1A patent/CN103734184A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5785867A (en) * | 1993-08-05 | 1998-07-28 | Nalco Chemical Company | Method and composition for inhibiting growth of microorganisms including peracetic acid and a non-oxidizing biocide |
| US20100078393A1 (en) * | 2008-10-01 | 2010-04-01 | Bei Yin | Biocidal compositions and methods of use |
| CN102783482A (en) * | 2011-05-19 | 2012-11-21 | 大连百傲化学有限公司 | 3-isothiazolinone composition |
Non-Patent Citations (4)
| Title |
|---|
| 刘春华等: "基于异噻唑啉酮的复合杀生剂的研究与分析", 《万方数据库》 * |
| 周晓霜等: "过氧化氢水溶液催化氧化环戊烯制备戊二醛", 《辽宁师范大学学报(自然科学版)》 * |
| 崔小明: "水处理杀生剂的研究开发进展", 《化工科技市场》 * |
| 薛晓茜等: "钨酸催化环戊烯氧化合成戊二醛条件的考察", 《辽宁科技大学学报》 * |
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Application publication date: 20140423 |