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A kind of preparation method of polyethylene glycol diazo polymer

A polyethylene glycol and polymer technology, applied in the field of ultraviolet photopolymerization, can solve the problems of poor coating stability and complex coating process, and achieve the effects of good repeatability, simple and fast preparation process, and simplified process.

Active Publication Date: 2017-03-08
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For this reason, the technical problem to be solved by the present invention is the problem that the existing capillary wall coating material coating process is complicated and the coating stability is poor, and then a kind of preparation method of polyethylene glycol diazo polymer is provided, described Under the action of the driving force of the syringe, the polyethylene glycol diazo polymer assembles and grows on the inner wall of the quartz capillary, and after ultraviolet light, the polyethylene glycol diazo polymer and the silicon hydroxyl group on the inner wall of the capillary undergo photocuring crosslinking reaction to form a coating

Method used

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  • A kind of preparation method of polyethylene glycol diazo polymer
  • A kind of preparation method of polyethylene glycol diazo polymer
  • A kind of preparation method of polyethylene glycol diazo polymer

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preparation example Construction

[0036] The preparation method of polyethylene glycol diazo polymer of the present invention comprises the following steps:

[0037] A kind of polyethylene glycol diazopolymer, it has structure shown in formula (1):

[0038]

[0039] Wherein n is an integer of 8-135.

[0040] Its synthesis process route is as follows:

[0041]

[0042] The method for activating the bare capillary column of the present invention comprises the steps:

[0043] successively use 0.1mol·L -1 Sodium hydroxide solution, distilled water, 0.1mol L -1 Salt

[0044] Rinse the bare capillary column with acid solution, distilled water and methanol for 30 min, 10 min, 30 min,

[0045] 10min and 10min, finally with N 2 Dry the bare capillary column to obtain an activated bare capillary column.

Embodiment 1

[0047] A preparation method of polyethylene glycol diazo polymer, comprising the steps of:

[0048] S1, synthesis of dichloropolyethylene glycol:

[0049] Put dried polyethylene glycol (PEG, molecular weight Mw of 400) and N,N-dimethylformamide (DMF) in a reaction kettle to form solution A; place thionyl chloride in a constant pressure dropping funnel middle,

[0050] To form solution B, add solution B drop by drop into solution A at 50°C until mixed evenly; the molar ratios of polyethylene glycol to N,N-dimethylformamide and thionyl chloride are respectively 1:2.0 and 1:3.0. After the mixed solution was reacted at 60°C under reflux for 20 hours, the product was washed with saturated brine, adjusted to pH 7.0 with anhydrous potassium carbonate, dried in vacuo to remove water, and filtered to remove sodium chloride to obtain the product dichloropolyethylene dichloride Alcohol (Cl-PEG-Cl);

[0051] S2, synthesis of amino-terminated phenyl polyethylene glycol:

[0052] P-ami...

Embodiment 2

[0060] A preparation method of polyethylene glycol diazo polymer, comprising the steps of:

[0061] S1, synthesis of dichloropolyethylene glycol:

[0062] Put dried polyethylene glycol (PEG, molecular weight Mw: 1000) and N,N-dimethylformamide (DMF) in a reaction kettle to form solution A; place thionyl chloride in a constant pressure dropping funnel , form B solution, and drop B solution into solution A drop by drop under the condition of 40°C until the mixture is uniform; the molar ratio of polyethylene glycol to N,N-dimethylformamide and thionyl chloride 1:1.5 and 1:2.0, respectively. After reacting the mixed solution at 85°C under reflux for 15 hours, the product was washed with saturated brine, adjusted to pH 7.0 with anhydrous potassium carbonate, dried in vacuo to remove water, and filtered to remove sodium chloride to obtain the product dichloropolyethylene dichloride Alcohol (Cl-PEG-Cl);

[0063] S2, synthesis of amino-terminated phenyl polyethylene glycol:

[006...

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Abstract

The invention relates to a polyethylene glycol diazonium polymer. The polyethylene glycol diazonium polymer is of a structure which is shown in a first image and is obtained through modified polyethylene glycol. After the polyethylene glycol diazonium polymer is illuminated by ultraviolet light, and photocuring and cross-linking reactions are carried on the polyethylene glycol diazonium polymer and silanol groups on the inner wall of a capillary tube to form a coating. The preparation of the coating can be conducted in an aqueous phase through a self-assembly mode, and the preparation process is simple and rapid. Chemical bonding of the coating is achieved through the photocuring and cross-linking reactions of the photonasty polyethylene glycol diazonium polymer, and quality problems such as capillary tube blocking are not prone to occurring.

Description

technical field [0001] The invention relates to the field of ultraviolet light polymerization, in particular to a preparation method of a polyethylene glycol diazo polymer, and the use of the polyethylene glycol diazo polymer to carry out electrostatic self-assembly and photocuring cross-linking reaction to form a stable Covalently bonded capillary coating. Background technique [0002] In recent years, capillary electrophoresis has been widely used in the fields of drug detection, life science, environmental protection and food inspection, especially in various It has been rapidly developed and widely used in the separation and analysis of biological macromolecules such as proteins and RNA. However, due to the electrostatic interaction, van der Waals force and hydrogen bond interaction between the unmodified capillary inner wall surface and the protein, non-specific adsorption occurs on the inner wall of the capillary, which affects the separation and analysis of proteins ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/338C08G65/325C08G65/333C08G65/332C09D171/00C03C17/32
Inventor 丛海林于冰陈新
Owner QINGDAO UNIV
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