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Preparation method of C21-36 alicyclic diisocyanate and use

A technology of diisocyanate and alicyclic diisocyanate, which is applied in the field of preparation of C21-36 alicyclic diisocyanate, can solve the problems of harsh process conditions, easy occurrence of side reactions, and difficulty in industrialization, achieves environmental friendliness, and is conducive to industrial popularization and application. , the effect of less production difficulty

Active Publication Date: 2013-05-22
陕西聚泰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the phosgene method is that the process conditions are harsh, the toxicity is high, it is not easy to industrialize, the yield is low, the side reaction is easy to occur, and it brings inconvenience to the post-treatment, such as the reaction between the generated isocyanate and the raw material amine
[0004] At present, the basic raw material selected for the preparation method of dibasic acid ester, an intermediate product of cycloaliphatic diisocyanate, is oleic acid or ester, which contains three double bonds, and easily produces by-products in the reaction preparation process, and the by-products The structure is similar, not easy to separate

Method used

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  • Preparation method of C21-36 alicyclic diisocyanate and use
  • Preparation method of C21-36 alicyclic diisocyanate and use
  • Preparation method of C21-36 alicyclic diisocyanate and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: Preparation of unsaturated cycloaliphatic dibasic acid (raw material A)

[0043] Add 1.7mol dehydrated ricinoleic acid ester, 1.7mol fatty acid methyl ester containing double bonds and 1.5g of hydroquinone as a polymerization inhibitor to a 2000mL pressure reactor, replace the air in the kettle with nitrogen, heat up to 160-180°C, and react The crude dibasic acid methyl ester was obtained in 3.5 hours. The above crude product was heated and refluxed at 80-90° C. for 4 hours with 680 mL of 10% sodium hydroxide solution in mass fraction, and acidified with hydrochloric acid with a mass fraction of 10%-15%. Saturated dibasic acid is distilled under reduced pressure to obtain a pure product, which is used as the basic raw material for preparing unsaturated alicyclic diisocyanate in subsequent examples, and its structural formula is shown in formula A:

[0044]

[0045] In the formula, x=1~7, R 1 , R 2 , R 3 for H atom or C 1-8 straight-chain or branched...

Embodiment 2

[0046] Embodiment 2: Preparation of unsaturated cycloaliphatic dibasic acid (raw material A)

[0047] The difference between this example and Example 1 is that the raw materials for preparing unsaturated alicyclic dibasic acids are different. In Example 1, esters are used to prepare acids, and in this example, acids are used to prepare acids.

[0048] Add 1.7mol of dehydrated ricinoleic acid and 1.7mol of double bond-containing fatty acid into a 2000mL pressure reactor, replace the air in the kettle with nitrogen, heat up to 160-180°C, react for 3.5 hours to obtain crude dibasic acid, and distill under reduced pressure to obtain pure As the basic raw material for preparing unsaturated cycloaliphatic diisocyanate in subsequent examples, its structural formula is shown in formula A.

Embodiment 3

[0049] Embodiment 3: Preparation of saturated alicyclic dibasic acid (raw material B)

[0050] Add the unsaturated aliphatic dibasic acid prepared in step embodiment 1 or embodiment 2 to another 2 liters of autoclave, add 500g methanol and 30g Pd (5%) / activated carbon catalyst (wet: dry weight 15g, 0.75g Pd), vacuumize, nitrogen replacement, hydrogen replacement respectively. The reaction mixture was stirred at 160-170° C., 1.5-2.0 Mp for about 7.5 hours, until the hydrogen absorption was complete, and the stirring was stopped. The material was filtered off under nitrogen pressure, leaving the catalyst in the filter. Use 500g of methanol to backwash the catalyst into the reactor, then add another part of the same unsaturated aliphatic dibasic acid, repeat the hydrogenation, the catalyst activity does not decrease, carry out the hydrogenation 5 times in the same way, and use the catalyst repeatedly for 4 Next, the obtained reaction mixture (colorless and transparent) is disti...

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Abstract

The invention provides a preparation method of C21-36 alicyclic diisocyanate and use. The preparation method comprises the following steps of: preparing an unsaturated alicyclic binary acid based on dehydrated ricinoleic acid or ester and a double bond containing fatty acid or ester as raw materials; preparing a saturated alicyclic binary acid through hydrogenation reaction; preparing acyl chloride of the alicyclic binary acid by acylating chlorination; preparing a trinitride of alicyclic binary acid by nitriding reaction; and finally preparing the alicyclic diisocyanate through isomerized decomposition reaction. According to the invention, acid or ester extracted from castor oil is used as a basic material, so that the production raw material is easy to get and low in cost, and prepared alicyclic diisocyanate is single in structure, less in side reaction and small in production difficulty, and the molecular weight is within a range of 300-500. According to the method, a same solvent is used in later three steps to the benefit of industrialization. The whole process is simple to operate, mild in condition, environment-friendly, safe in production, and is very beneficial for industrial popularization and application.

Description

technical field [0001] The present invention relates to a class of alicyclic diisocyanates, in particular to a C 21-36 Preparation method and use of cycloaliphatic diisocyanate. Background technique [0002] Isocyanate is a substance with high reactivity, especially diisocyanate is a kind of substance that is used in a huge amount in the field of material industry. At present, toluene diisocyanate (TDI) is used in the largest amount, but due to the high toxicity of aromatic diisocyanate, Even the degradation products are relatively toxic and carcinogenic, and the pollution in the production process is relatively large, and the materials made of it are easy to yellow, so people turn their attention to alicyclic diisocyanate and isophorone diisocyanate. (IPDI) is one of them, but due to its small molecular weight and relatively high volatility, IPDI has relatively high inhalation toxicity. Therefore, people have been searching for less toxic or even non-toxic aliphatic diisoc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/14C07C263/12
CPCY02P20/584
Inventor 刘林学张明英赵彬侠李建民
Owner 陕西聚泰新材料科技有限公司
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