Preparation method for temperature-sensitive fine particle surface-grafted cross-linked complex gel

A technology of surface grafting and composite gel is applied in the field of preparation of temperature-sensitive microsphere surface grafting and cross-linked composite gel, which can solve the problems of complicated operation, low product purity, poor toughness and the like, and achieves simple operation and high product quality. The effect of high purity and good mechanical properties

Inactive Publication Date: 2017-05-31
SHAANXI YIPINDA PETROCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the response characteristics of this type of gel are affected by the relaxation of polymer segments and the restriction of the three-dimensional gel network structure, the response speed is relatively slow.
At the same time, the mechanical strength of the gel, especially the poor toughness, greatly limits its application.
[0003] In recent years, there have been many studies on the construction of high-strength gels based on the grafting and cross-linking of polymer microspheres or inorganic particles, combined with physical interactions such as hydrogen bonds, electrostatic interactions, and dipole interactions, but the operations are complicated and the purity of the products is low. , which limits its wide application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation method of temperature-sensitive type microsphere surface graft cross-linked composite gel comprises the following steps:

[0018] (1) Preparation of microparticles:

[0019] Dissolve 15g of N-vinylformamide in 500mL of aqueous solution, heat to 70°C, and then add 1g of azobisisobutylamidine hydrochloride to initiate aqueous polymerization to obtain polymerized N-vinylformamide. After adding 200mL of 1mol / L NaOH solution, react at 90°C for 3 hours to generate polyvinylamine, add 0.68g N'-isopropylacrylamide, 0.43g butyl methacrylate and 0.28g polyvinylamine in sequence, add 100mL water, adjust the pH of the solution Adjust the value to 7~8, pass N 2 After 30 minutes, add 0.60 g of tert-butyl hydroperoxide aqueous solution with a mass fraction of 0.1%, stir and react in a heating oil bath at 70°C for 6 hours, and naturally cool to room temperature after the reaction to obtain a microparticle emulsion;

[0020] (2) Preparation of composite hydrogel:

[...

Embodiment 2

[0023] The preparation method of temperature-sensitive type microsphere surface graft cross-linked composite gel comprises the following steps:

[0024] (1) Preparation of microparticles:

[0025] Dissolve 15g of N-vinylformamide in 500mL of aqueous solution, heat to 70°C, and then add 1g of azobisisobutylamidine hydrochloride to initiate aqueous polymerization to obtain polymerized N-vinylformamide. After adding 200mL of 1mol / L NaOH solution, react at 90°C for 3 hours to generate polyvinylamine, add 0.68g N'-isopropylacrylamide, 0.43g butyl methacrylate and 0.28g polyvinylamine in sequence, add 100mL water, adjust the pH of the solution Adjust the value to 7~8, pass N 2 After 30 minutes, add 0.60 g of tert-butyl hydroperoxide aqueous solution with a mass fraction of 0.1%, stir and react in a heating oil bath at 70°C for 6 hours, and naturally cool to room temperature after the reaction to obtain a microparticle emulsion;

[0026] (2) Preparation of composite hydrogel:

[...

Embodiment 3

[0029] The preparation method of temperature-sensitive type microsphere surface graft cross-linked composite gel comprises the following steps:

[0030] (1) Preparation of microparticles:

[0031] Dissolve 15g of N-vinylformamide in 500mL of aqueous solution, heat to 70°C, and then add 1g of azobisisobutylamidine hydrochloride to initiate aqueous polymerization to obtain polymerized N-vinylformamide. After adding 200mL of 1mol / L NaOH solution, react at 90°C for 3 hours to generate polyvinylamine, add 0.68g N'-isopropylacrylamide, 0.43g butyl methacrylate and 0.28g polyvinylamine in sequence, add 100mL water, adjust the pH of the solution Adjust the value to 7~8, pass N 2 After 30 min, where, N 2 The flow rate is 10mL / min, add 0.60 g of tert-butyl hydroperoxide aqueous solution with a mass fraction of 0.1%, stir and react in a heating oil bath at 70°C for 6 hours, wherein the stirring speed is 250 rpm, and naturally cool to At room temperature, microparticle emulsion is ob...

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PUM

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Abstract

The invention discloses a preparation method for temperature-sensitive fine particle surface-grafted cross-linked complex gel. The preparation method comprises the following steps: (1) fine particle preparation: preparing fine particle emulsion from N-vinylformamide, water, azobisisobutryamide chloride, a NaOH solution, N'-isopropylacrylamide, butyl methacrylate, polyvinylamine and a tert-butyl hydroperoxide aqueous solution serving as raw materials; (2) preparing a complex gel sample from N'-isopropylacrylamide, the fine particle emulsion prepared in the step (1) and a tert-butyl hydroperoxide aqueous solution serving as raw materials, and soaking the complex gel sample in distilled water to obtain the temperature-sensitive fine particle surface-grafted cross-linked complex gel. The preparation method is easy to operate; the prepared product has high purity; the prepared complex gel has high mechanical performance, and has high sensitivity to the temperature.

Description

technical field [0001] The invention belongs to the field of gel preparation, and in particular relates to a preparation method of temperature-sensitive microsphere surface grafted and cross-linked composite gel. Background technique [0002] Smart gels are a class of special functional materials that change in response to external stimuli (such as pH, light, electricity, magnetism, temperature, etc.). The stimuli responsiveness of traditional smart gels generally comes from the changes in the gel network structure caused by the stressful changes in the polymer chain structure or functional groups in the three-dimensional network, such as those based on the hydrophobic association between hydrophobic side chains. Hydrophobic association cross-linked physical gel. Polyelectrolyte gels based on electrostatic interactions between ionized groups on side chains, etc. However, because the response characteristics of this type of gel are affected by the relaxation of polymer chai...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C08F285/00C08F271/00C08F220/54C08F220/18C08F8/00C08F126/02
CPCC08F8/00C08F271/00C08F285/00C08F126/02C08F220/54C08F220/1804
Inventor李长英
OwnerSHAANXI YIPINDA PETROCHEM CO LTD