CN103351313A - Preparation process for xylylene diisocyanate - Google Patents
Preparation process for xylylene diisocyanate Download PDFInfo
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- CN103351313A CN103351313A CN2013102714139A CN201310271413A CN103351313A CN 103351313 A CN103351313 A CN 103351313A CN 2013102714139 A CN2013102714139 A CN 2013102714139A CN 201310271413 A CN201310271413 A CN 201310271413A CN 103351313 A CN103351313 A CN 103351313A
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- xylylene diisocyanate
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Abstract
The invention specifically discloses a preparation process for xylylene diisocyanate, which belongs to the technical field of synthetic materials. The preparation process comprises the following steps: 1, with bis(trichloromethyl)carbonate and hydrochloride in a mass ratio of 1: 1.5-3 as reaction raw materials, controlling temperature to be -10 to 40 DEG C, introducing carbon dioxide, carrying out stirring for 15 to 30 m, then carrying out cooling and adding an inertial organic solution; 2, heating a reaction solution for a reaction, wherein air pressure is 0.1 to 1 Mpa and heating temperature is 60 to 100 DEG C; and 3, subjecting a prepared reaction solution to pressure reduction, filtration and distillation so as to obtain xylylene diisocyanate. The preparation process for xylylene diisocyanate provided by the invention overcomes the problems of low processing and synthesis efficiency, low purity and a complex method in the prior art and can rapidly and easily process and synthesize xylylene diisocyanate with high purity; meanwhile, the price of equipment used in processing and synthesis is moderate, so needs for processing and synthesis of middle and small-sized enterprises are met, and production cost investment of the enterprises is reduced.
Description
Technical field
The present invention relates to the synthetic materials technical field, be specifically related to a kind of preparation technology for xylylene diisocyanate.
Background technology
Known from institute, xylylene diisocyanate (being called for short XDI), to be oxidized to highland diformazan wing by mixing hexichol (71% m-xylene and 29% p-Xylol) with oxygen, hydrogenating reduction becomes benzene dicarbonitrile, phosgenation is made again, it is widely used in the processing of various coating, resin etc., is main chemical industry synthesis material.
Existing xylylene diisocyanate is synthetic generally to adopt light phosgenation to make, raw materials consumption was well large and synthesis device is expensive when it synthesized on the one hand, the processing combined coefficient is low, purity is low, and there is certain risk in the excessive poisonous phosgene of employing in complicated, the not easily separated and preparation process of synthetic reaction process; Synthetic employed equipment price is expensive on the other hand, and production cost drops into higher, can't satisfy medium-sized and small enterprises and process synthetic demand.
Therefore, based on the problems referred to above, the invention provides a kind of preparation technology for xylylene diisocyanate.
Summary of the invention
Goal of the invention: the object of the invention is for overcoming above-mentioned the deficiencies in the prior art, a kind of preparation technology for xylylene diisocyanate is provided, can greatly improve synthetic production efficiency, sintetics purity on the one hand, synthetic employed equipment price is moderate on the other hand, can satisfy the medium-sized and small enterprises requirement.
Technical scheme: the invention provides a kind of preparation technology for xylylene diisocyanate, comprise with
Lower step,
Step 1, be that two (trichloromethyl) carbonic ethers of 1:1.5-3 and hydrochloride are former as reaction with mass ratio
Material is controlled at subzero 10 ℃-40 ℃ with temperature, passes into carbonic acid gas and stirs 15m-30m, adds inert organic solvent after the cooling.
Step 2, the reaction soln of step 1 is carried out reacting by heating, air pressure 0.1Mpa-1Mpa wherein, 60 ℃-100 ℃ of Heating temperatures, the reaction times is 2.5h-3.5h.
After reducing pressure, filter, distill, step 3, the reaction soln that step 2 is made namely get xylylene diisocyanate.
Temperature is subzero 5 ℃-30 ℃ in the preferred described step 1, passes into carbonic acid gas and stirs 20m-25m.
The inert organic solvent that adds in the preferred described step 1 is the mixture of chlorobenzene, Meta Dichlorobenzene, toluene or its composition.
Reaction pressure 0.3Mpa-0.8Mpa in the preferred described step 2,70 ℃-90 ℃ of Heating temperatures, the reaction times is 2.8h-3h.
Distillation time is 15m-30m in the preferred described step 3.
Compared with prior art, beneficial effect of the present invention is:
A kind of preparation technology for xylylene diisocyanate of the present invention, solved that existing processing combined coefficient is low, purity is low and method is complicated problem, can be fast, simple processing synthesizes the high xylylene diisocyanate of purity; The synthetic employed equipment price of simultaneously processing is moderate, has satisfied the synthetic needs of medium-sized and small enterprises processing, has reduced enterprise's production cost and has dropped into.
Embodiment
Below in conjunction with specific embodiment a kind of preparation technology for xylylene diisocyanate of the present invention is elaborated:
The invention provides a kind of preparation technology for xylylene diisocyanate, may further comprise the steps,
Step 1, be that two (trichloromethyl) carbonic ethers of 1:1.5-3 and hydrochloride are former as reaction with mass ratio
Material is controlled at subzero 10 ℃-40 ℃ with temperature, passes into carbonic acid gas and stirs 15m-30m, adds inert organic solvent after the cooling.
Step 2, the reaction soln of step 1 is carried out reacting by heating, air pressure 0.1Mpa-1Mpa wherein, 60 ℃-100 ℃ of Heating temperatures, the reaction times is 2.5h-3.5h.
After reducing pressure, filter, distill, step 3, the reaction soln that step 2 is made namely get xylylene diisocyanate.
Temperature is subzero 5 ℃-30 ℃ in the preferred step 1, passes into carbonic acid gas and stirs 20m-25m.
The inert organic solvent that adds in the preferred step 1 is the mixture of chlorobenzene, Meta Dichlorobenzene, toluene or its composition.
Reaction pressure 0.3Mpa-0.8Mpa in the preferred step 2,70 ℃-90 ℃ of Heating temperatures, the reaction times is 2.8h-3h.
Distillation time is 15m-30m in the preferred step 3.
The above only is preferred implementation of the present invention, should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also make some improvement, and these improvement also should be considered as protection scope of the present invention.
Claims (5)
1. preparation technology who is used for xylylene diisocyanate is characterized in that: may further comprise the steps,
Step 1, with mass ratio be two (trichloromethyl) carbonic ethers of 1:1.5-3 and hydrochloride as reaction raw materials, will
Temperature is controlled at subzero 10 ℃-40 ℃, passes into carbonic acid gas and stirs 15m-30m, adds inert organic solvent after the cooling;
Step 2, the reaction soln of step 1 is carried out reacting by heating, air pressure 0.1Mpa-1Mpa wherein, 60 ℃-100 ℃ of Heating temperatures, the reaction times is 2.5h-3.5h;
After reducing pressure, filter, distill, step 3, the reaction soln that step 2 is made namely get xylylene diisocyanate.
2. a kind of preparation technology for xylylene diisocyanate according to claim 1, it is characterized in that: temperature is subzero 5 ℃-30 ℃ in the described step 1, passes into carbonic acid gas and stirs 20m-25m.
3. a kind of preparation technology for xylylene diisocyanate according to claim 1 is characterized in that: the inert organic solvent that adds in the described step 1 is the mixture of chlorobenzene, Meta Dichlorobenzene, toluene or its composition.
4. a kind of preparation technology for xylylene diisocyanate according to claim 1 is characterized in that: reaction pressure 0.3Mpa-0.8Mpa in the described step 2, and 70 ℃-90 ℃ of Heating temperatures, the reaction times is 2.8h-3h.
5. a kind of preparation technology for xylylene diisocyanate according to claim 1, it is characterized in that: distillation time is 15m-30m in the described step 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102714139A CN103351313A (en) | 2013-07-01 | 2013-07-01 | Preparation process for xylylene diisocyanate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013102714139A CN103351313A (en) | 2013-07-01 | 2013-07-01 | Preparation process for xylylene diisocyanate |
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| CN103351313A true CN103351313A (en) | 2013-10-16 |
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| CN2013102714139A Pending CN103351313A (en) | 2013-07-01 | 2013-07-01 | Preparation process for xylylene diisocyanate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5740451A (en) * | 1980-08-22 | 1982-03-06 | Mitsui Toatsu Chem Inc | Preparation of organic isocyanate by two-stage process comprising cooling and heating steps |
| EP0384463A1 (en) * | 1989-02-23 | 1990-08-29 | MITSUI TOATSU CHEMICALS, Inc. | Preparation process of xylylene diisocyanate |
| EP0492145A2 (en) * | 1990-12-20 | 1992-07-01 | Mitsubishi Gas Chemical Company, Inc. | Process for producing xylylene diisocyanate |
| CN1931834A (en) * | 2005-09-13 | 2007-03-21 | 杭州崇舜化学有限公司 | Synthesis process of phenyl dimethylene diisocyanate |
| CN102070491A (en) * | 2010-11-26 | 2011-05-25 | 烟台万华聚氨酯股份有限公司 | Method for preparing xylylene diisocyanate based on salification-phosgenation reaction |
-
2013
- 2013-07-01 CN CN2013102714139A patent/CN103351313A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5740451A (en) * | 1980-08-22 | 1982-03-06 | Mitsui Toatsu Chem Inc | Preparation of organic isocyanate by two-stage process comprising cooling and heating steps |
| EP0384463A1 (en) * | 1989-02-23 | 1990-08-29 | MITSUI TOATSU CHEMICALS, Inc. | Preparation process of xylylene diisocyanate |
| EP0492145A2 (en) * | 1990-12-20 | 1992-07-01 | Mitsubishi Gas Chemical Company, Inc. | Process for producing xylylene diisocyanate |
| JPH04221356A (en) * | 1990-12-20 | 1992-08-11 | Mitsubishi Gas Chem Co Inc | Production of xylylene diisocyanate |
| CN1931834A (en) * | 2005-09-13 | 2007-03-21 | 杭州崇舜化学有限公司 | Synthesis process of phenyl dimethylene diisocyanate |
| CN102070491A (en) * | 2010-11-26 | 2011-05-25 | 烟台万华聚氨酯股份有限公司 | Method for preparing xylylene diisocyanate based on salification-phosgenation reaction |
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Application publication date: 20131016 |