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A kind of preparation method and application of 10-hydroxyl-1,8-diazabicycloundeca-7-ene

A diazabicyclo, hydroxyl technology, applied in the field of polyurethane, can solve the problems of no catalytic gel, high-efficiency catalyst, low activity, etc.

Active Publication Date: 2017-08-11
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity of the reaction-type catalysts obtained so far is generally lower than that of traditional catalysts, and there is no high-efficiency catalyst that can specifically focus on catalytic gels

Method used

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  • A kind of preparation method and application of 10-hydroxyl-1,8-diazabicycloundeca-7-ene
  • A kind of preparation method and application of 10-hydroxyl-1,8-diazabicycloundeca-7-ene
  • A kind of preparation method and application of 10-hydroxyl-1,8-diazabicycloundeca-7-ene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Carrier 1: Preparation of Mn-ZSM-5 molecular sieve

[0081] Weigh 40g of dried ZSM-5 molecular sieve (silicon-aluminum ratio 30-40); weigh 1.2g of manganese sulfate, dissolve it in 60ml of pure water, and prepare a manganese sulfate solution, and pour the solution into the above-mentioned ZSM-5 molecular sieve , after stirring evenly, let stand for 12h, dry at 120°C, and activate at 550°C for 4h to obtain the modified Mn-ZSM-5 molecular sieve.

[0082] Step 1: Heat 60g caprolactam, 2g potassium ethoxide and 100ml ethanol to boiling, add 50ml epichlorohydrin dropwise within 30min, reflux for 1h, cool to room temperature, add 6ml6N sulfuric acid to acidify, filter, evaporate ethanol, and then The fraction at 201-205°C was collected under reduced pressure (7mmHg), which was N-(3-chloro-2-hydroxypropyl)caprolactam, and the yield was 89.2% according to gas chromatography. The product was qualitatively analyzed by mass spectrometry and NMR. Figure see Figure 2-4 .

[0083...

Embodiment 2

[0085] Carrier one: with reference to embodiment 1

[0086] Step 1: Heat 60g of caprolactam, 4g of potassium ethylate and 100ml of isopropanol to boiling, add 50ml of epichlorohydrin dropwise within 30min, reflux for 2.5h, cool to room temperature, add 6ml of 6N sulfuric acid to acidify, filter, and evaporate the isopropanol After alcohol, the fraction at 201-205°C was collected under reduced pressure (7mmHg), which was N-(3-chloro-2-hydroxypropyl)caprolactam, with a yield of 90.9%.

[0087] Step 2: Add 35g of N-(3-chloro-2-hydroxypropyl) caprolactam and 1.75g ​​of the ZSM-5 molecular sieve prepared above into the reaction kettle, after nitrogen replacement, add 100ml of dioxane containing 47g of liquid ammonia The temperature of the solution was raised to 80°C, and after stirring for 1.5 hours, nitrogen gas was blown into it to purge for 30 minutes, and the catalyst was filtered out. Then add 500ml of water, filter, dry, and collect fractions at 145-150°C under a pressure of...

Embodiment 3

[0089] Carrier one: with reference to embodiment 1

[0090] Step 1: Heat 60g caprolactam, 0.3g potassium ethoxide and 100ml isopropanol to boiling, add 50ml epichlorohydrin dropwise within 30min, reflux for 1h, cool to room temperature, add 6ml6N sulfuric acid to acidify, filter, and evaporate ethanol , and then collect the fraction at 201-205° C. under reduced pressure (7 mmHg), which is N-(3-chloro-2-hydroxypropyl) caprolactam, with a yield of 83%.

[0091] Step 2: Add 20g of N-(3-chloro-2-hydroxypropyl)caprolactam and 1.75g ​​of the ZSM-5 molecular sieve prepared above into the reaction kettle, after nitrogen replacement, add 100ml of liquid ammonia, heat up to 80°C, and stir After 1.5h, the pressure was released, and ethanol was added to filter out the catalyst. After the ethanol was distilled off, the fraction collected at 145-150°C under a pressure of 7 mmHg was 10-hydroxy-1,8-diazabicycloundec-7-ene with a yield of 92.1%.

[0092] The raw materials that comparative ex...

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Abstract

The present invention provides a preparation method and uses of 10-hydroxy-1,8-diazabicycloundec-7-ene. The preparation method comprises that: (1) caprolactam and epichlorohydrin are subjected to addition in the presence of an alkaline catalyst (1) to generate N-(3-chloro-2-hydroxypropyl)caprolactam; and (2) the N-(3-chloro-2-hydroxypropyl)caprolactam and an ammonia-containing solution are subjected to a dehydration condensation reaction in the presence of a catalyst (2) to generate the 10-hydroxy-1,8-diazabicycloundec-7-ene. The present invention further provides a combination material capable of being used for producing polyurethane foam with characteristics of low odor and low VOC, and polyurethane foam produced by using the combination material. Compared with the conventional polyurethane combination material, the combination material of the present invention has characteristics of good fluidity, rapid aging and the like. In addition, the prepared polyurethane foam has characteristics of substantially reduced VOC content, substantially reduced odor and good physical property.

Description

technical field [0001] The invention relates to a method for preparing 10-hydroxyl-1,8-diazabicycloundec-7-ene, which is a method for preparing 10-hydroxyl-1,8-ene by using caprolactam and epichlorohydrin as raw materials. - A method for diazabicycloundec-7-ene and its use in the field of polyurethanes. The invention also provides a composite material which can be used for producing low-odor and low-VOC polyurethane foam. Background technique [0002] As the country and society have higher and higher requirements for environmental protection and quality of life, polyurethane foam materials are more and more widely used in automotive interiors and home furnishing, and the requirements for environmental protection and odor are also getting higher and higher. Flexible polyurethane foams are generally produced by reacting isocyanates with polyols containing at least two isocyanate-compatible hydroxyl groups in the presence of catalysts, blowing agents and customary auxiliaries ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04C08G18/20
CPCC07D487/04C08G18/2072
Inventor 周明星李付国傅佳艺齐旺顺华卫琦
Owner WANHUA CHEM GRP CO LTD