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Method for preparing conjugated microporous polymer TiO2 composite nano antibacterial agent by in-situ method

A nano-antibacterial agent and conjugated micropore technology, which is applied in the field of in-situ preparation of conjugated microporous polymer TiO2 composite nano-antibacterial agent, can solve the problems of accelerated bacterial inactivation, bacterial inactivation, and low solar energy utilization rate. Achieve the effects of accelerating bacterial inactivation, widening the band gap, and improving photocatalytic antibacterial activity

Pending Publication Date: 2021-06-08
QIQIHAR UNIVERSITY
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Problems solved by technology

[0006] Aiming at the deficiencies of the prior art, the present invention provides an in-situ method for preparing conjugated microporous polymer TiO 2 The method of composite nano-antibacterial agent has the effect of broadening the TiO 2 bandgap, thereby improving the photocatalytic antibacterial activity of the composite material, accelerating the inactivation of bacteria and other advantages, solving the problem of TiO 2 The band gap is narrow, which is 3.2eV, and it can only absorb ultraviolet light with a short wavelength, so the utilization rate of solar energy is low, and the problem that bacteria cannot be inactivated in a short time

Method used

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  • Method for preparing conjugated microporous polymer TiO2 composite nano antibacterial agent by in-situ method

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preparation example Construction

[0033] see Figure 1-2 , the invention provides a conjugated microporous polymer TiO 2 The preparation method of composite nano antibacterial agent comprises the following steps:

[0034] S1. Ultrasonic dispersion of TiO in toluene 2 particles to disperse evenly.

[0035] S2. Preparation of conjugated microporous polymer / TiO 2 Composite nano antibacterial agent

[0036] S21, take 4,4'-diethynyl biphenyl, 2,4,6-tribromobenzoic acid, CuI, Pd(PPh 3 ) 2 Cl 2 and PPh 3 Placed in a three-necked flask; 4,4'-diethynyl biphenyl, 2,4,6-tribromobenzoic acid, CuI, Pd(PPh 3 ) 2 Cl 2 、PPh 3 and TiO 2 The mixing mass ratio is 20-22:24-26:1:2-4:12-14:350-450; the specific preferred mass ratio is 21:25:1:3:13:400, combining 4,4'- Diethynyl biphenyl with functional monomers having carboxyl groups and TiO 2 One-pot fabrication of conjugated microporous polymer / TiO by in situ polymerization 2 Composite nano antibacterial agent, wherein, the total mass of 4,4'-diethynyl biphenyl and...

Embodiment 1

[0042] (1) Take TiO 2 (4390mg, 54.94mmol) was added to a beaker containing 20mL of toluene, and ultrasonically oscillated for 1h.

[0043] (2) Take 4,4'-diethynylbiphenyl (202mg, 1.00mmol), 2,4,6-tribromobenzoic acid (239mg, 0.67mmol), CuI (9.52mg, 50μmol), Pd(PPh 3 ) 2 Cl 2 (35.12 mg, 100 μmol) and PPh 3 (131mg, 500μmol) was placed in a 250ml three-necked bottle.

[0044] (3) Under the protection of nitrogen, inject toluene (10.00mL) and triethylamine (15.00mL) into (2), and add the mixture in (1) in (2), stir well, and the mixture is heated to 85°C, and stirred at 85°C for 36 hours to obtain a mixed solid powder.

[0045] (4) The solid powder obtained in (3) was washed three times with chloroform, toluene and saturated potassium iodide aqueous solution respectively, and then the solid powder was Soxhlet-extracted for 72 hours with dichloromethane as a solvent.

[0046] (5) Dry the solid powder extracted from (4) at 50°C for 12 hours to constant weight to obtain a conju...

Embodiment 2

[0048] (1) Take TiO 2 (4190mg, 49.94mmol) was added into a beaker containing 20mL of toluene, and ultrasonically oscillated for 2h.

[0049] (2) Take 4,4'-diethynylbiphenyl (180mg, 0.80mmol), 2,4,6-tribromobenzoic acid (190mg, 0.465mmol), CuI (7.52mg, 40μmol), Pd(PPh 3 ) 2 Cl 2 (45.12mg, 80μmol) and PPh 3 (120mg, 450μmol) was placed in a 250ml three-necked bottle.

[0050] (3) Under the protection of nitrogen, inject toluene (8.00mL) and triethylamine (13.00mL) into (2), and add the mixture in (1) in (2), stir well, the mixture is heated to 85°C and stirred at 90°C for 36 hours to obtain a mixed solid powder.

[0051] (4) The solid powder obtained in (3) was washed three times with chloroform, toluene and saturated potassium iodide aqueous solution respectively, and then the solid powder was Soxhlet-extracted for 72 hours with dichloromethane as a solvent.

[0052] (5) Dry the solid powder extracted from (4) at 50°C for 12 hours to constant weight to obtain a conjugated ...

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Abstract

The invention belongs to the technical field of TiO2 composite materials, and discloses a method for preparing a conjugated microporous polymer TiO2 composite nano antibacterial agent by an in-situ method. The method comprises the following steps: ultrasonically dispersing TiO2 particles: adding a certain amount of TiO2 into a beaker containing toluene, sealing the beaker by using a preservative film, and putting the sealed beaker into an ultrasonic cleaner for oscillation to obtain a mixture A; adding 4, 4 '-diethynyl biphenyl, 2, 4, 6-tribromobenzoic acid, CuI, Pd (PPh3) 2Cl2 and PPh3 into a three-necked bottle filled with triethylamine and methylbenzene; according to the method for preparing the conjugated microporous polymer TiO2 composite nano antibacterial agent, the TiO2 particles grow on the surface and inside of a conjugated microporous polymer in an in-situ polymerization mode, the conjugated microporous polymer has the characteristics of high stability, high hydrophobicity, high photon activity and the like, the band gap of TiO2 can be effectively widened, and the antibacterial property of the conjugated microporous polymer is improved. Therefore, the photocatalytic antibacterial activity of the composite material is improved, and bacterial inactivation is accelerated.

Description

technical field [0001] The present invention relates to TiO 2 The technical field of composite materials, specifically an in-situ method for preparing conjugated microporous polymer TiO 2 The method of composite nano antibacterial agent. Background technique [0002] In recent decades, human activities have become increasingly frequent, causing more and more serious bacterial pollution, which poses a serious threat to human health and the ecological environment. The emergence of antibiotic-multidrug-resistant bacteria is considered one of the major challenges facing modern public health. [0003] Microbial contamination has become the main way for the transmission of infectious diseases, usually these pollutants have good solubility in water, can penetrate deep soil and reach groundwater. Among the many sterilization processes, chlorine gas, chlorine dioxide gas and ozone gas are the most effective sterilizing agents for killing most microorganisms, but these gases are to...

Claims

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Application Information

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IPC IPC(8): C08G61/10C08K3/22A61L2/08
CPCC08G61/10C08K3/22A61L2/088C08G2261/12C08G2261/1426C08G2261/312C08G2261/411C08K2201/011C08K2003/2241C08G2261/18
Inventor 藏雨吴云峰徐亮荆博宇
Owner QIQIHAR UNIVERSITY
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