Process for preparing polyisocyanate by solid phosgene

A polyisocyanate and solid phosgene technology, which is applied in the preparation of isocyanate derivatives, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of cumbersome process, complicated post-treatment and purification process, and insufficient color and mechanical properties of isocyanate polyurethane. Meet the use requirements and other issues

A polyisocyanate and solid phosgene technology, which is applied in the preparation of isocyanate derivatives, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of cumbersome process, complicated post-treatment and purification process, and insufficient color and mechanical properties of isocyanate polyurethane. Meet the use requirements and other issues

CN1827593AInactive Publication Date: 2006-09-06北京金源化学集团有限公司
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Lysine Triisocyanate (LTI):

[0019] Add 449.6g (4.31mol) 35% HCl solution in 1L four-necked flask and dropwise add 167.2g (2.74mol) ethanolamine in 30 minutes, add 250.0g (1.37mol) lysine hydrochloride after dropwise addition, and The reaction was stirred at 45°C for 10 minutes. The temperature was raised to 110°C, the pressure was reduced to 4KPa, and the water in the reaction system was evaporated. After returning to normal pressure, HCl gas was passed through to react for 3 hours, and then the water was evaporated under reduced pressure. This process is repeated several times, and the reaction is stopped after lysine hydrochloride is consumed, and o-dichlorobenzene (ODCB) and methanol are added to crystallize, and the crystal is washed several times with ODCB to obtain lysine aminoethyl ester trihydrochloride (LAET) .

[0020] The 2500ml reactor is equipped with mechanical stirring and two sets of dripping devices. Add 100ml o-dichlorobenzene (ODCB) in the react...

Embodiment 2

[0022] Lysine Triisocyanate (LTI):

[0023] Except that bis-(trichloromethyl)carbonate is changed into 445.5g (1.5mol), other reaction conditions are the same as embodiment 1, obtain LTI content 68.6% (HPLC) in the product, NCO content 40.3wt% (theoretical value 47.2wt%) %), HCl content 0.70wt%, ODCB content 0.81wt%.

Embodiment 3

[0025] Lysine Triisocyanate (LTI):

[0026] Except that bis-(trichloromethyl) carbonate is changed to 891g (3mol), other reaction conditions are the same as in Example 1, and LTI content 86.3% (HPLC) is obtained in the product, NCO content 43.6wt% (theoretical value 47.2wt%) , HCl content 0.35wt%, ODCB content 0.31wt%.

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Abstract

The invention relates to a method for preparation of 1, 2-dialkoxy-3-fluorobenzene by an intermediate of 2-fluorin-6-halogenated phenol. The said method consists of selecting 2-fluorophenol as its stock, and obtaining the intermediate of 2-fluorin-6-halogenated phenol; afterwards, performing multiple steps such as etherifing the said intermediate and etherifing again by introducing the hydroxyl group, alternatively, hydroxylating and etherifing the said intermediate; finally, obtaining the said 1, 2-dialkoxy-3-fluorobenzene. The method is of low cost, high yield rate, so it is suitable for the industrial production.

Description

technical field [0001] The invention relates to a method for preparing polyisocyanate by using solid phosgene and polyamine or its salt. Background technique [0002] Isocyanates are commonly used in the preparation of polyurethane resins, coatings and adhesives. As we all know, polyurethane has a wide range of applications in optical materials, automotive and construction materials, sealing materials, and daily necessities due to its good mechanical properties. In addition, polyisocyanates and polyurethane resins prepared from amino acids, such as lysine, can be used in biomedicine due to their good biocompatibility. [0003] Current methods for preparing isocyanates generally utilize the reaction of phosgene with amines. In patents US5,136,086, US4,419,295, JP2002-003462, JP06-234722, CN1125718A, CN1197793A, CN1516688A and EP424836, phosgene is used to phosgenate amines to prepare isocyanates. However, there are many problems in this method due to the use of phosgene. F...

Claims

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Application Information

Patent Timeline
06 Sep 2006
Publication
CN1827593A
IPC
C07C265/14; C07C263/10
Inventors
邱明建; 张炜