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Synthesis method of dimer(fatty acid)yl diisocyanate

A technology for dimerization of fatty acid diisocyanate and synthesis method, which is applied in the preparation of carboxylic acid nitrogen-containing derivatives, organic chemistry, etc., can solve problems such as low yield, and achieve the effect of high total yield

Inactive Publication Date: 2010-09-15
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But the yield of this method is low, and its yield is 56.11~62.35%

Method used

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  • Synthesis method of dimer(fatty acid)yl diisocyanate
  • Synthesis method of dimer(fatty acid)yl diisocyanate
  • Synthesis method of dimer(fatty acid)yl diisocyanate

Examples

Experimental program
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Effect test

Embodiment 1

[0018] (1) 400ml of toluene solution containing 112.40g (0.20mol) of dimerized tall oleic acid and 5g of catalyst dimethylformamide were respectively added to a 1000ml reaction flask with a thermometer and a dropping funnel, and stirred at a temperature of 70°C. 150ml of toluene solution dissolved with 29.70g (0.10mol) of bis(trichloromethyl) carbonate was added dropwise under the state, and the reaction was continued for 1 hour after the dropwise addition, cooled to room temperature, filtered, and after toluene was evaporated, 114.76g of dichloromethane was obtained. Polytall oleic acid chloride;

[0019] (2) 54.58g (0.42mol) of sodium azide and 120ml of deionized water were respectively added to a 1000ml reaction flask with a thermometer placed on an ice-water bath, and the solution was added dropwise at a temperature of 10°C under stirring. There is a 200 ml acetone solution of 114.76 g of dimerized tall oil acid chloride obtained in step (1), after the dropwise addition of...

Embodiment 2

[0032] (1) The method is the same as in Example 1, except that the reaction temperature in step (1) is 80° C., and the bis (trichloromethyl) carbonate is 19.80 g (0.067 mol) to obtain 115.12 g of dimerized tall oil acid. acid chloride;

[0033] (2) method is with embodiment 1, and the difference is that the sodium azide in step (2) is 49.78g (0.394mol);

[0034] (3) The method is the same as that in Example 1, except that the reaction temperature in step (3) is 70° C. to obtain 81.12 g of a brown-red transparent oily liquid with a total yield of 72.95%.

Embodiment 3

[0036] (1) The method is the same as in Example 1, except that the reaction temperature in step (1) is 75° C., and the bis (trichloromethyl) carbonate is 25.74 g (0.087 mol) to obtain 116.81 g of dimerized tall oil. acid chloride;

[0037] (2) method is with embodiment 1, and the difference is that the sodium azide in step (2) is 52.03g (0.41mol);

[0038] (3) The method is the same as that in Example 1, except that the reaction temperature in step (3) is 67° C. to obtain 84.52 g of a brown-red transparent oily liquid with a total yield of 76.01%.

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Abstract

The invention discloses a synthesis method of dimer(fatty acid)yl diisocyanate, which comprises the steps of: adding a methylbenzene solution of dimer(tall oil acid) and dimethylformamide into a reaction bulb, dropping a methylbenzene solution containing di(trichloromethyl) carbonic ester under the stirring at a temperature of 70-80 DEG C, reacting for 1h, filtering, evaporating to remove methylbenzene to obtain dimer(tall oil acid) acyl chloride, wherein the mol ratio of the dimer(tall oil acid) to the di(trichloromethyl) carbonic ester is 3:1-1.5; adding sodium azide and deionized water into the reaction bulb, dropping an acetone solution dissolved with the dimer(tall oil acid) acyl chloride under the stirring, adding 300ml of normal hexane, dimixing, washing a normal hexane layer by using cold water, drying by using anhydrous sodium sulfate to obtain an anhydrous sodium sulfate solution of dimer(tall oil acid) acyl azide, wherein the mol ratio of the dimer(tall oil acid) acyl chloride to the sodium azide is 1:2-2.2; and adding 300ml of normal hexane into the reaction bulb, dropping the normal hexane solution under the stirring at a temperature of 65-70 DEG C, and continuing to react for 30min after the dropping to obtain a target product.

Description

technical field [0001] The invention relates to a method for synthesizing dimerized fatty acid diisocyanate, in particular to a method for synthesizing dimerized tall oil diisocyanate. Background technique [0002] Dimeric fatty acid diisocyanate (DDI) is an aliphatic isocyanate with a molecular structure of thirty-six carbons (prepared by sodium azide method) or thirty-eight carbons (prepared by amination method). DDI reacts with active hydrogen-containing compounds at a slower rate than other isocyanates such as toluene-2,4-diisocyanate (TDI), isocyanatomethyl-3,5,-5-trimethylcyclohexylisocyanate (IPDI) and condensed Diurea triisocyanate (N-100), considered a harmless isocyanate. Therefore, DDI is not only widely used in civil industries such as coatings, inks, and waterproofing agents, but also has a wide range of uses in the military field. It can be used as a curing agent for propellant binders and thermal insulation layers of rocket engines. [0003] At present, ther...

Claims

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Application Information

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IPC IPC(8): C07C265/14C07C263/12
Inventor 王晗樊学忠聂天明蔚红建刘晓刚李吉祯张伟付小龙黄小梧梁勇封利民范明辉
Owner XIAN MODERN CHEM RES INST
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