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Preparation method of isophorone diamidoformate

A technology of isophorone dicarbamate and isophorone diamine, which is applied in the field of preparation of isophorone dicarbamate, can solve the problems of increasing production cost, expensive ionic liquid and the like, and achieves the Simple operation, easy separation and recycling, mild reaction conditions

Active Publication Date: 2014-09-17
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent 02158320.X discloses a synthesis method of ammonia and dimethyl carbonate, which uses ionic liquid as solvent and catalyst system, and is characterized by high reactivity, easy operation, easy product separation and catalyst recovery, but ionic liquid is expensive , which increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method of isophorone dicarbamate, its specific steps are:

[0026] (1) Add isophorone diamine dropwise to the mixed system of dimethyl carbonate and supported solid catalyst, react at 50°C for 16 hours, and filter; among them, dimethyl carbonate is 27 g, isophorone diamine 17.0g, 0.88g supported solid catalyst.

[0027] (2) Add 3 times the volume of distilled water to the filtered filtrate, stand still, filter, and dry to obtain 24.7 g of isophorone dicarbamate with a yield of 86.3% and a purity of 97.1%.

[0028] The specific preparation method of the supported solid catalyst is:

[0029] (1) 33.1g Pb(NO 3 ) 2 Dissolved in water, phosphoric acid adjusts the pH to 3;

[0030] (2) Add 423.7g of carrier silica to the above aqueous solution, immerse at room temperature for 2 hours, dry at 110°C for 6 hours, and calcinate at 580°C for 3 hours to obtain a supported solid catalyst PbO / SiO 2 , The active component loading is 5wt%.

Embodiment 2

[0032] A preparation method of isophorone dicarbamate, its specific steps are:

[0033] (1) Add isophorone diamine dropwise to the mixed system of dimethyl carbonate and supported solid catalyst, react at 55°C for 12 hours, and filter; among them, dimethyl carbonate is 90g, isophorone diamine 17.0g, supported solid catalyst 10.7g.

[0034] (2) Add 10 times the volume of distilled water to the filtered filtrate, stand still, filter, and dry to obtain 25.3 g of isophorone dicarbamate with a yield of 88.5% and a purity of 98.2%.

[0035] The specific preparation method of the supported solid catalyst is:

[0036] (1) 33.1g Pb(NO 3 ) 2 Dissolved in water, phosphoric acid adjusts the pH to 3.1;

[0037] (2) Add 52g of carrier alumina to the above aqueous solution, immerse at room temperature for 2.5 hours, dry at 100°C for 4 hours, and calcinate at 450°C for 5 hours to obtain a supported solid catalyst PbO / Al 2 O 3 , The active component loading is 30wt%.

Embodiment 3

[0039] A preparation method of isophorone dicarbamate, its specific steps are:

[0040] (1) Add isophorone diamine dropwise to the mixed system of dimethyl carbonate and supported solid catalyst, react at 60°C for 9 hours, and filter; among them, dimethyl carbonate is 54 g, isophorone two Amine 17.0g, supported solid catalyst 4.26g.

[0041] (2) Add 6 times the volume of distilled water to the filtered filtrate, stand still, filter, and dry to obtain 25.0 g of isophorone dicarbamate with a yield of 87.3% and a purity of 96.8%.

[0042] The specific preparation method of the supported solid catalyst is:

[0043] (1) Add 29.7g Zn (NO 3 ) 2 ·6H 2 O is soluble in water, and phosphoric acid adjusts the pH to 3.2;

[0044] (2) Add 32.56g of carrier silica to the above aqueous solution, immerse at room temperature for 3 hours, dry at 110°C for 8 hours, and calcinate at 480°C for 4 hours to obtain a supported solid catalyst ZnO / SiO 2 , The active component loading is 20wt%.

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Abstract

The invention relates to a preparation method of isophorone diamidoformate. The method comprises the following steps: getting dimethyl carbonate and isophorone diamine as the raw materials; and catalyzing the raw materials to react by virtue of a loaded solid catalyst; and then separating by distilled water so as to obtain the product that is the isophorone diamidoformate. The method is free from hypertoxic phosgene, environmentally-friendly, and mild in reaction condition, can be carried out at medium and low temperature, and brings simple requirements to equipment; the catalyst can be conveniently separated and recycled; and the product is separated by adding the distilled water, and the rectification is saved, so that the operation is simple and convenient, and the purity of the product is higher.

Description

Technical field [0001] The invention relates to a preparation method of isophorone dicarbamate, which adopts a supported solid catalyst and uses distilled water to precipitate the product in post-treatment. Background technique [0002] Isophorone dicarbamate (IPDC) is an important intermediate for the production of isophorone diisocyanate (IPDI), and IPDI is one of the important raw materials for the production of polyurethane. IPDI is the most versatile diisocyanate. It is compatible with almost all resins and all solvents. It has large molecular weight, low toxicity, good weather resistance, not easy to yellow, reasonable price, and long service life. Compared with other isocyanates, it is resistant Thermal performance is better. [0003] The traditional method of producing diisocyanates is the phosgene method. The amine phosgenation method is a traditional industrial production method for synthesizing IPDI, and it is also the most industrialized production method currently. H...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C271/24C07C269/04B01J23/14B01J23/06
Inventor 白君君牟庆平门振张建林高洪奎栾波马韵升史庆苓
Owner CHAMBROAD CHEM IND RES INST CO LTD