CN1160297C - Method and apparatus for continuous synthesis of vinyl isobutyl ether - Google Patents
Method and apparatus for continuous synthesis of vinyl isobutyl ether Download PDFInfo
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- CN1160297C CN1160297C CNB021382859A CN02138285A CN1160297C CN 1160297 C CN1160297 C CN 1160297C CN B021382859 A CNB021382859 A CN B021382859A CN 02138285 A CN02138285 A CN 02138285A CN 1160297 C CN1160297 C CN 1160297C
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Abstract
The present invention relates to a method for synthesizing vinylisobutyl ether by a continuous method, which comprises that mixing gas of ethyne and nitrogen and isobutanol are used as raw materials of the reaction; an etherification reaction is carried out in an etherification tower; the mixing gas of the ethyne and the nitrogen are introduced from the bottom of the etherification tower; the isobutanol and catalyst solution are sprayed from the upper part of the etherification tower; the mixing gas of the ethyne and the nitrogen reversely contacts the isobutanol in the etherification tower to make the etherification reaction; the temperature of the etherification reaction is from 130 to 160 DEG C; the pressure of the etherification tower is from 0.38 to 0.65MPa; the vinylisobutyl ether generated from the reaction and the unreacted mixing gas of the ethyne and the nitrogen are led out from the top of the etherification tower and enter a receiving tank after passing through a condenser; the unreacted mixing gas of the ethyne and the nitrogen continues to be recovered and used. The conversion rate per pass of the ethyne of the present invention can reach more than 57%, and the yield of a synthesis reaction is more than 95 %.
Description
Technical field
The present invention relates to the continuous processing etherification technology, especially the continuous processing etherificate generates the synthetic method and the device thereof of vinyl isobutyl ether.
Background technology
Vinyl isobutyl ether is the main raw material of polymerization chlorinated polyether resin (LMP resin), and the resin that chlorinated polyether resin is taken the lead in developing by companies such as BASF still belongs to blank as the vinyl isobutyl ether of main raw material at home.Chlorinated polyether resin as coating, it is the base-material of protective system, compare with protective system resins such as chlorinated rubber, chlorinatedpolyethylene, chlorosulfonated polyethylenes, chlorinated polyether resin (LMP resin) excellent water tolerance and chemical resistant properties, photostabilization, be difficult for being atmospheric oxidn, with all kinds of metal substrates excellent sticking power is arranged all, identical character with other chlorine-containing polymer protective system is arranged, and solvability is good, therefore has than better effect of chlorinated rubber and range of application.
The etherification technology of vinyl isobutyl ether yet there are no the more detailed bibliographical information that continuous processing is produced, and the continuous processing etherification technology obviously can obtain the better product of quality and productive rate.
Summary of the invention
The objective of the invention is: a kind of etherification technology of vinyl isobutyl ether is provided, and especially the continuous processing production technique makes it have better processing condition and good quality, enhances productivity, guarantees the subsequent product quality.
The object of the present invention is achieved like this: with acetylene and nitrogen mixture and isopropylcarbinol is reaction raw materials, in the etherificate tower, carry out etherification reaction, acetylene and nitrogen mixture feed from the etherificate tower bottom, isopropylcarbinol and catalyst solution make acetylene carry out etherification reaction with nitrogen mixture with isopropylcarbinol reverse contact in the etherificate tower by the top spray of etherificate tower.The temperature of etherification reaction is 130-160 ℃, the pressure 0.38-0.65Mpa of etherificate tower.The concentration of acetylene and nitrogen mixture: acetylene content 30-60%, catalyzer are the solution that contains KOH, and content is 8-16%.Vinyl isobutyl ether that reaction generates and unreacted acetylene and nitrogen mixture are derived by the etherificate cat head, and enter receiver behind condenser.The feeding amount (amounting to into acetylene) of acetylene and nitrogen mixture: isopropylcarbinol 8-18Kg/min, 2-5kg/min, catalyzer KOH 0.5-2kg/min.The content of acetylene (weight) is below 60% in acetylene and the nitrogen mixture.
Characteristics of the present invention are: under condition of the present invention, be suitable for the continuous processing etherification technology and produce vinyl isobutyl ether.The present invention and custom-designed device can make the per pass conversion of acetylene can reach 57%, and the yield of building-up reactions is at (in acetylene) more than 95%.Technological reaction of the present invention is steady, and processing parameter control is simple, and unit consumption is low, and the production environment cleaning is to produce vinyl isobutyl ether technology preferably.
Description of drawings
Fig. 1 is apparatus of the present invention structural representation
Hydraucone N1, catalyzer relief outlet N2, cat head gaseous phase outlet N4, cat head side gas backstreaming outlet N3, liquid inlet N5, the tower bottom side also is provided with circulating liquid mouth N7.Circulating liquid input and output mouth S1, S2
Embodiment
Specific embodiments of the invention are as follows:
Acetylene and nitrogen mixture evenly feed from the etherificate tower bottom, isopropylcarbinol and catalyst solution are evenly sprayed by the top of etherificate tower, acetylene is fully contacted in the etherificate tower with isopropylcarbinol with nitrogen mixture, the vinyl isobutyl ether that reaction generates is continuously steamed by the etherificate tower, unreacted acetylene and nitrogen mixture should continue to reclaim use, the per pass conversion of this device acetylene can reach more than 57%, and the yield of building-up reactions is at (in acetylene) more than 95%.
Technical process:
Behind lyophilization, enter one section inlet of acetylene compressor from the acetylene gas of Acetylene Gas Holder, the compressor outlet place that is compressed in by acetylene compressor is mixed with nitrogen, the content of acetylene all can 30%, 40%, 50% in the gas mixture, gas mixture enters drying tower, in drying tower, further purified, entered the etherificate tower then.
Etherification reaction, inject isopropylcarbinol-catalyst solution in the etherificate tower in advance, this catalyst solution is by conveying systemic circulation inside and outside tower of pump, acetylene gas constantly feeds from the bottom of etherificate tower, isopropylcarbinol-catalyst solution makes acetylene fully contact in the etherificate tower with isopropylcarbinol with nitrogen mixture by etherificate tower top spray.The temperature of reaction of control regulation and the pressure of system, the temperature of etherification reaction be 130.5,145,160 ℃ all feasible, the pressure of etherificate tower is slightly fluctuation in reaction, because reaction is thermopositive reaction, is controlled at 0.38-0.65Mpa easily by controls such as flows.Etherification reaction is constantly carried out.Systemic circulation by material is in time taken away reaction heat.Vinyl isobutyl ether that reaction generates and unreacted acetylene and nitrogen mixture are derived by the etherificate cat head, and enter receiver behind condenser.Isolate vinyl isobutyl ether and unreacted acetylene and nitrogen mixture simultaneously, derive vinyl isobutyl ether liquefaction back, and unreacted acetylene and nitrogen mixture continue to participate in reaction.Yield is respectively at 93%, 95%, 94% (in acetylene).
When feeding acetylene and nitrogen mixture to the etherificate tower, simultaneously by pump constantly to etherificate tower fresh makeup catalyst.The catalyzer of inactivation is regularly discharged, and life of catalyst is more than 1000 hours; Recycling of tail gas, acetylene per pass conversion of the present invention is between 50-57%.Through unreacted acetylene after the etherificate tower two outlets are arranged: one is that the inlet of getting back to acetylene compressor directly enters the etherificate tower and recycles, and another outlet is with N-Methyl pyrrolidone acetylene gas to be absorbed, then desorb.
Reclaim the acetylene in the tail gas, the utilization ratio of acetylene gas is reached more than 95%, and reduced topsoil, the acetylene content of exhaust emissions is below 0.5%.
The acetylene per pass conversion is (in acetylene) between 50-57%
Catalyst concn (KOH content): 8-16%
The norm quota of consumption of main raw material(s) (vinyl isobutyl ether per ton):
Acetylene 310Kg, isopropylcarbinol 920Kg, 210 cubic metres of nitrogen, catalyzer KOH100kg
The synthesizer that the continuous processing etherificate generates vinyl isobutyl ether also claims the etherificate tower, the withstand voltage tower body of circular metal, tower height is at 8-20 rice, tower diameter is provided with gas upwards and enters hydraucone N1 at 0.5-1 rice at the bottom of the tower, the tower bottom side is provided with catalyzer relief outlet N2, cat head N4 is a gaseous phase outlet, the cat head side is provided with gas backstreaming outlet N5, and the top of tower also is provided with circulating liquid input aperture N3, and the tower bottom side also is provided with circulating liquid mouth N7.
In Fig. 1, present embodiment be tower height at 12 meters, tower diameter is at 0.6 meter, the gas hydraucone N1 that makes progress in the tower directly is .0.35 rice.The upper liquid input aperture N5 of tower is below cat head side gas backstreaming outlet N3, and tower bottom side catalyzer relief outlet N2 is concordant substantially with the position that the tower bottom side also is provided with circulating liquid mouth N7.
Claims (5)
1. the method for continuous synthesis of vinyl isobutyl ether, with acetylene and nitrogen mixture and isopropylcarbinol is reaction raw materials, in the etherificate tower, carry out etherification reaction, it is characterized in that acetylene and nitrogen mixture feed from the etherificate tower bottom, isopropylcarbinol and catalyst solution are by the top spray of etherificate tower, make acetylene carry out etherification reaction with isopropylcarbinol reverse contact in the etherificate tower with nitrogen mixture, the concentration of acetylene and nitrogen mixture: acetylene content 30-60%, catalyzer is the solution that contains KOH, content is 8-16%, the temperature of etherification reaction is 130-160 ℃, the pressure 0.38-0.65Mpa of etherificate tower, vinyl isobutyl ether that reaction generates and unreacted acetylene and nitrogen mixture are derived by the etherificate cat head, and enter receiver behind condenser.
2. by the method for the described continuous synthesis of vinyl isobutyl ether of claim 1, it is characterized in that through unreacted acetylene after the etherificate tower two outlets being arranged: one is that the inlet of getting back to acetylene compressor directly enters the etherificate tower and recycles, another outlet is with N-Methyl pyrrolidone acetylene gas to be absorbed, desorb then, acetylene gas is recycled.
3. by the method for the described continuous synthesis of vinyl isobutyl ether of claim 1, the feeding amount that it is characterized in that acetylene and nitrogen mixture is amounted to into the acetylene meter: isopropylcarbinol 8-18Kg/min, 2-5kg/min, catalyzer KOH0.5-2kg/min, the content of acetylene is at 30-60% in acetylene and the nitrogen mixture.
4. the continuous processing etherificate generates the synthesizer of vinyl isobutyl ether, it is characterized in that the withstand voltage tower body of circular metal, tower height is at 8-20 rice, tower diameter is provided with gas upwards and enters hydraucone (N1) at 0.5-1 rice at the bottom of the tower, the tower bottom side is provided with catalyzer relief outlet (N2), cat head (N4) is a gaseous phase outlet, the cat head side is provided with gas backstreaming outlet (N5), and the top of tower also is provided with circulating liquid input aperture (N3), and the tower bottom side also is provided with circulating liquid mouth (N7).
5. generated the synthesizer of vinyl isobutyl ether by the described continuous processing etherificate of claim 5, it is characterized in that 12 meters of tower heights, tower diameter is at 0.6 meter, and gas hydraucone (N1) footpath that makes progress in the tower is 0.35 meter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021382859A CN1160297C (en) | 2002-09-17 | 2002-09-17 | Method and apparatus for continuous synthesis of vinyl isobutyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021382859A CN1160297C (en) | 2002-09-17 | 2002-09-17 | Method and apparatus for continuous synthesis of vinyl isobutyl ether |
Publications (2)
| Publication Number | Publication Date |
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| CN1401619A CN1401619A (en) | 2003-03-12 |
| CN1160297C true CN1160297C (en) | 2004-08-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021382859A Expired - Fee Related CN1160297C (en) | 2002-09-17 | 2002-09-17 | Method and apparatus for continuous synthesis of vinyl isobutyl ether |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555198B (en) * | 2008-07-10 | 2014-01-15 | 杭州电化集团有限公司 | Synthesis method of isobutyl vinyl ether and device thereof |
| CN101898939B (en) * | 2010-08-06 | 2012-05-02 | 安陆新景化工有限公司 | Method for preparing compound 4-hydroxy butyl vinyl ether |
| CN102807479A (en) * | 2011-06-03 | 2012-12-05 | 焦作新景科技有限公司 | Method for synthesizing vinyl cyclohexyl ether |
| CN102701920B (en) * | 2012-05-29 | 2015-03-18 | 浙江锦华新材料股份有限公司 | Method for purifying vinyl isobutyl ether |
| CN110433759B (en) * | 2019-09-03 | 2024-04-05 | 湖北襄化机械设备有限公司 | Synthetic tower for vinyl methyl ether |
| CN115043734B (en) * | 2022-07-26 | 2024-07-19 | 山东奥友生物科技股份有限公司 | Continuous production process of 2,4 '-trichloro-2' -nitrodiphenyl ether |
| CN115974657A (en) * | 2022-12-06 | 2023-04-18 | 浙江皇马科技股份有限公司 | Process method and system for preparing vinyl ether by reaction of high-boiling-point monohydric alcohol and acetylene |
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- 2002-09-17 CN CNB021382859A patent/CN1160297C/en not_active Expired - Fee Related
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| CN1401619A (en) | 2003-03-12 |
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