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Method for preparing elastomer based on Click reaction

An elastomer and reaction technology, applied in the field of new materials, can solve the problems of long-time heating and slow speed, and achieve the effects of good mechanical properties, simple preparation process and great application value

Active Publication Date: 2012-09-12
碳衡(重庆)生物质新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the other hand, the rate of this cycloaddition reaction is relatively slow, and for unactivated alkynes (non-electron-deficient and strain-free), it usually requires prolonged heating

Method used

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  • Method for preparing elastomer based on Click reaction
  • Method for preparing elastomer based on Click reaction
  • Method for preparing elastomer based on Click reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of preparation method based on the elastomer of Click reaction, it comprises the steps:

[0038] 1) Preparation of alkynylated polybutadiene: Hydroxyl-terminated polybutadiene (HTPB, i.e., butylated hydroxyl) was vacuum-dried at 50 oC for 2 h; the hydroxyl-terminated polybutadiene with a hydroxyl value of 0.8399 mmol KOH / g was weighed Dissolve 10.52g of alkenes in 20mL of THF to obtain a THF solution containing HTPB; another 2.16g of potassium tert-butoxide (t-BuOK) was dissolved in 20mL of THF to obtain a t-BuOK solution; Slowly add the THF solution containing HTPB into the t-BuOK solution, and continue to stir for 10 minutes to obtain the reaction solution A; take 2.4mL of propargyl bromide (80% w / w, ca. 9.2mol / L) and dissolve it in 60mL of THF [The total amount of —OH in hydroxyl-terminated polybutadiene (HTPB, ie, butylated hydroxyl group): Potassium tert-butoxide (t-BuOK): the molar ratio of propyne bromide=1:2.2:2.5], in N 2 Under the conditions of protect...

Embodiment 2

[0045] A kind of preparation method based on the elastomer of Click reaction, it comprises the steps:

[0046] 1) Preparation of alkynylated polybutadiene: Hydroxyl-terminated polybutadiene (HTPB, i.e., butylated hydroxyl) was vacuum-dried at 50 oC for 2 h; the hydroxyl-terminated polybutadiene with a hydroxyl value of 0.8399 mmol KOH / g was weighed 10.98g of alkenes was dissolved in 20mL of THF to obtain a THF solution containing HTPB; another 2.08g of potassium tert-butoxide (t-BuOK) was dissolved in 20mL of THF to obtain a t-BuOK solution; Slowly add the THF solution containing HTPB into the t-BuOK solution, and continue to stir for 10 min to obtain the reaction solution A; take 2.0 mL of propargyl bromide (80% w / w, ca. 9.2 mol / L) and dissolve it in 100 mL of THF [The total amount of —OH in hydroxyl-terminated polybutadiene (HTPB, ie, butylated hydroxyl group): Potassium tert-butoxide (t-BuOK): the molar ratio of propyne bromide=1:2.0:2.0], in N 2 Under the conditions of pr...

Embodiment 3

[0053] A kind of preparation method based on the elastomer of Click reaction, it comprises the steps:

[0054] 1) Preparation of alkynylated polybutadiene: Hydroxyl-terminated polybutadiene (HTPB, i.e., butylated hydroxyl) was vacuum-dried at 50 oC for 2 h; the hydroxyl-terminated polybutadiene with a hydroxyl value of 0.8399 mmol KOH / g was weighed 10.96g of alkenes was dissolved in 20mL of THF to obtain a THF solution containing HTPB; another 2.08g of potassium tert-butoxide (t-BuOK) was dissolved in 20mL of THF to obtain a t-BuOK solution; Slowly add the THF solution containing HTPB into the t-BuOK solution, and continue to stir for 10 min to obtain the reaction solution A; take 2.0 mL of propargyl bromide (80% w / w, ca. 9.2 mol / L) and dissolve it in 100 mL of THF [The total amount of —OH in hydroxyl-terminated polybutadiene (HTPB, ie, butylated hydroxyl group): Potassium tert-butoxide (t-BuOK): the molar ratio of propyne bromide=1:2.0:2.0], in N 2 Under the conditions of pr...

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Abstract

The invention relates to a method for preparing elastomer based on Click reaction. The method for preparing elastomer based on the Click reaction is characterized by including the steps: 1) preparing alkynylation polybutadiene; 2) according to the molar ratio of the total quantity of alkynylation polybutadiene end-C Xi C to N3 in glycidyl azide polymer to cuprous halides being 1:1-4:0.05-0.5, dissolving the alkynylation polybutadiene and the glycidyl azide polymer in tetrahydrofuran, adding glycidyl azide polymer solution into alkynylation polybutadiene solution to obtain mixed solution M, adding the cuprous halides into the mixed solution M under the condition of N2 protection and stirring, keeping the temperature at 0-25 DEG C, and performing reaction away from light for 8-24h to obtainreaction solution N; and 3) performing suction filtration for the reaction solution N, drying filtrate with anhydrous MgSO4, and performing filtration, concentration and solvent volatilization to obtain the elastomer based on the Click reaction. The preparation process is simple, and the elastomer prepared by the method has a good mechanical property.

Description

technical field [0001] The invention relates to a method for preparing an elastomer based on Click reaction, and belongs to the technical field of new materials. Background technique [0002] In recent years, the application of 1,3-dipolar cycloaddition (1,3-dipolar cycloaddition, also known as Click reaction) in the construction of new cross-linked network structures has attracted widespread attention at home and abroad. Compared with the curing reaction of the polyurethane system, the curing using this type of Click reaction is not sensitive to moisture in the environment, so there is no need to take measures such as dehumidification (such as drying of fillers) during the reaction process. Moreover, since the chemical potential energies of the azide compounds and alkynes involved in the reaction are relatively high, they have the special property of thermodynamic instability, which will cause them to emit more than 188 kJ / mol energy. On the other hand, the rate of this c...

Claims

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Application Information

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IPC IPC(8): C08G81/02
Inventor 黄进丁有朝胡冲章桥新余家会
Owner 碳衡(重庆)生物质新材料有限公司
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