Macromolecular bactericide and method for preparation

A technology of bactericide and polymer, applied in the field of polymer bactericide and its preparation, can solve rare problems and achieve the effect of good killing microorganism effect.

Active Publication Date: 2005-07-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, there are few reports on the direct modification of hyperbranched polymers to synthesize hyperbranched polymer fungicides

Method used

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  • Macromolecular bactericide and method for preparation
  • Macromolecular bactericide and method for preparation
  • Macromolecular bactericide and method for preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This embodiment is the preparation of chlorobutyryl chloride.

[0042] Add 40mL of thionyl chloride and 3g of anhydrous zinc chloride into a 150mL 3-neck round bottom flask equipped with mechanical stirring, start stirring, and quickly add 38mL of γ-butyrolactone to raise the temperature of the solution to 45°C. The reaction mixture was heated to 55°C and the reaction was stirred for 22 hours. The supernatant was transferred to a 150 mL round-bottomed flask for rotary vacuum evaporation and separation. The unreacted raw materials were evaporated at a residual pressure of 3 mmHg and a temperature of 80° C., and the obtained liquid was chlorobutyryl chloride.

[0043] 13 CNMR ( figure 1 ) characterization only appears the following characteristic peaks: δ173.20 (ClCOCH 2 CH 2 CH 2 Cl), δ46.43(ClCOCH 2 CH 2 CH 2 Cl), δ27.8(ClCOCH 2 CH 2 CH 2 Cl), δ44.53(ClCOCH 2 CH 2 CH 2 Cl), indicating that chlorobutyryl chloride has been obtained.

Embodiment 2

[0045] This embodiment is the preparation of the intermediate product HP2Cl.

[0046] Add 100mL tetrahydrofuran and 20.0g BoltornH20 into a 250mL 3-neck round bottom flask equipped with mechanical stirring, start stirring, and add 29.9mL pyridine after the solid is dissolved. Slowly add 41.5mL of chlorobutyryl chloride dropwise in an ice-water bath, and react at room temperature for 24 hours after the dropwise addition, pour the reaction mixture into 1L of deionized water, a brown viscous solid precipitates, and then dissolves the precipitate in acetone , poured into 1L deionized water, and repeated 3 times. The obtained brown viscous solid was vacuum-dried at a residual pressure of 3 mmHg and a temperature of 80°C. 29.5 g of product were obtained (75.0% yield). Through element analysis, the product contains Cl 16.60% (weight).

[0047] From 1 H NMR analysis shows that raw material Boltorn H 20 ( figure 2 ) of two hydroxyl characteristic peaks, δ4.94 (CH 2 OH) and δ3.46...

Embodiment 3

[0049] This embodiment is the preparation of the final product HP2N12.

[0050] Add 30.0mL dimethyl sulfoxide and 5.0gHP2Cl into a 150mL 3-neck round bottom flask equipped with mechanical stirring, start stirring, and add 12.6mL dodecyldimethyl tertiary amine (Jiangsu Feixiang Chemical Co., Ltd. product). Reacted at 80°C for 48 hours, cooled to room temperature, poured the reaction mixture into 300mL acetone, a light brown solid precipitated, then dissolved the precipitate in ethanol, poured into 300mL acetone, repeated 3 times. The obtained brown solid was vacuum-dried at a residual pressure of 3 mmHg and a temperature of 80° C. to obtain 6.3 g of the product (yield 63.0% by weight). Through elemental analysis, the product contains 3.22% (weight) of N.

[0051] From 1 H NMR analysis shows that after the quaternization reaction (product HP N , Figure 4 ), HP2Cl ( image 3 ) The characteristic peak of δ3.64 disappears, and δ3.05 (CH 2 NCH 2 C 10 h 20 CH 3 ), δ1.23 (N...

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Abstract

A macromolecule bactericide has the following structure: as shown in the right formula, HP represents the frame of hyperbranched polymers, n is an integer between 1 and 8, z is the result of 2n+1, R is -O-CO-CH2-CH2-CH2-, -O-CO-CH2-CH2-, -O-CO-CH2-, -O-CO-NH-CH2-CH2-CH2-, -O-CO-NH-CH2-CH2- or -O-CO-NH-CH2-, Y is an alkyl whose carbon atom number is between 1 and 30, A and B are alkyls whose carbon atom number is between 1 and 4, X is an anion selected from Cl-íóBr-íóI-íóNO3-íóClO4-íóClO3-. The macromolecule bactericide provided by the invention can be obtained by quaternised modification of the end hydroxyl group of hyberbranched polymers. Compared with the quaternary ammonium salt bactericide, the bactericide has better effect to kill microbe when used for water containing system, its capability of killing Gram-negative bacteria is ten times as strong as that of the dodecyl trimethyl ammonium chloride. íí

Description

technical field [0001] The invention relates to a water treatment agent, in particular to a polymer bactericide for inhibiting microbial contamination in water systems and a preparation method thereof. technical background [0002] Since German Domak G discovered that quaternary ammonium salts containing long-chain alkyl groups have fungicidal activity in 1935, the synthesis of cationic fungicides has been one of the more active areas of fungicide research. At present, cationic fungicides have been widely used in the control of bacteria and algae in the process of industrial and civil water treatment, and in the sterilization and disinfection of medical and sanitation fields. When a fungicide is often used, microorganisms can develop drug resistance, so people are constantly synthesizing fungicides with new structures, and high-efficiency and rapid bactericidal performance is also what people expect new fungicides to have. [0003] In recent years, with the development of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N33/02C08G63/685
Inventor 刘杰李本高汪燮卿
Owner CHINA PETROLEUM & CHEM CORP
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