CN102304020A - Method for synthesizing pinacol by absorbing 2,3-dimethyl-2-butene with molecular sieve - Google Patents
Method for synthesizing pinacol by absorbing 2,3-dimethyl-2-butene with molecular sieve Download PDFInfo
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- CN102304020A CN102304020A CN201010566944A CN201010566944A CN102304020A CN 102304020 A CN102304020 A CN 102304020A CN 201010566944 A CN201010566944 A CN 201010566944A CN 201010566944 A CN201010566944 A CN 201010566944A CN 102304020 A CN102304020 A CN 102304020A
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Abstract
The invention discloses a method for synthesizing pinacol by absorbing 2,3-dimethyl-2-butene with a molecular sieve. The invention discloses a method for synthesizing high-purity pinacol product by using butane, hydrogen and air as raw materials and using platinum-palladium-osmium as a catalyst. The method is to react the mixture of 2,3-dimethyl-2-butene, hydrogen and air raw material at 100 to 150 DEG C under a reaction pressure of 0.2 to 0.5Mpa in the presence of a platinum-palladium-osmium catalyst. In the synthesis method disclosed by the invention, the catalyst has high activity, can be used repeatedly and is free from toxic, the reaction speed is mild, the reaction time is short, the yield is high, and pollution is avoided.
Description
Technical field
With butylene, hydrogen, sky is the gas raw material, and adopts platinum-palladium-osmium to make catalyzer, synthesizes highly purified pinacol product.
Background technology
It is raw material that the production technique of present domestic synthetic pinacol mainly adopts with acetone, makes catalyzer with mercuric acetate or mercury chloride, and after polymerization obtains again behind magnesium metal reduction.But this production technique cost is high, and yield is low, and productive rate is merely about 49%, and toxicity is big, and environmental pollution is serious.
Though there is the expert to adopt the synthetic pinacol of electrochemical method reduction acetone to overcome the drawback of chemical method to a certain extent.It is to be negative electrode with ZN-PTFE combined electrode, electrosynthesis pinacol in alkaline medium, but its productive rate also only reaches 53.6%, and a little more than the productive rate of chemical method preparation, productive rate is still lower.
Summary of the invention
The method of the synthetic pinacol that the present invention relates to has overcome the shortcoming of aforesaid method, provide a kind of catalyst activity high, can reuse, nontoxic and speed of response is gentle, the reaction times is shorter, yield height and free of contamination compound method.
Technical scheme of the present invention is just 2; 3 dimethyl--2-butylene, hydrogen, air feed the molecular sieve reaction tower respectively after being heated to 70 ℃-120 ℃ mixes; Make mixture under 100 ℃-150 ℃ temperature; 0.2-0.5Mpa reaction pressure under, under the effect of the platinum-palladium-osmium catalyst series of molecular sieve adsorption, react.
The present invention be a kind of catalyst activity high, can reuse, nontoxic and speed of response is gentle, the reaction times lacks, high, the free of contamination compound method of yield.Shown in its beneficial effect table specific as follows:
Two kinds of production process effects are following:
| Sequence number | Project | Acetone method | The butylene method |
| 1 | Catalyst activity | Higher | High |
| 2 | Catalyzer work-ing life | Reuse 5-6 time | Reuse |
| 3 | Catalyst toxicity | Poisonous | Nontoxic |
| 4 | Speed of response | Acutely, be prone to blast | Inviolent |
| 5 | Yield | 49% | 90% |
| 6 | The environmental protection aspect | Pollute bigger | Pollution-free |
Description of drawings
Fig. 1 is an artwork
Label among the figure:
1 condensing surface, 2 butylene grooves, 3 air compressor machines, 4 butylene well heaters
5 butylene surge tanks, 6 molecular sieve reaction towers, 7 product scoops, 8 hydrogen well heaters
9 hydrogen basins, 10 airheaters, 11 hydrogen gas buffers, 12 air cushioning jars
13 thermal oil oil heaters, 14 surge tanks, 15 rectifying stills, 16 scoops
17 condensing towers.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
Open air compressor machine 3; Air is compressed to 0.4-0.8Mpa; Feed the preheating of air internals preheating in the molecular sieve reaction tower 6, get into airheater 10 then and heat, until air heating to 70 ℃-120 ℃; Get into air cushioning jar 12 again and cushion, air pressure is transferred to 0.2-0.5Mpa; With 2,3 dimethyl--2-butylene is from 2, the 3 dimethyl--2-butylene preheating internals preheating of butylene groove 2 in being pumped into molecular sieve reaction tower 6, get into butylene well heater 4 then and heat; With 2; 3 dimethyl--2-butylene is heated to 70 ℃-120 ℃, gets into 2,3 dimethyl--2-butylene surge tank 5 again and cushions; 2,3 dimethyl--2-butylene pressure is transferred to 0.2-0.5Mpa; Hydrogen gets into the hydrogen preheating internals preheating in the molecular sieve reaction tower 6 from hydrogen basin 9 (the storage tank top hole pressure of hydrogen is transferred to 0.4-0.8Mpa); Getting into hydrogen well heater 8 then heats; Hydrogen is heated to 70 ℃-120 ℃; Get into hydrogen gas buffer 11 again and cushion, hydrogen pressure is transferred to 0.2-0.5Mpa.The mol ratio of material is 2,3 dimethyl--2-butylene: hydrogen: air=1.1:1:6.After each item preheating work is accomplished, the butylene that gasifies with 10m
3The flow of/h, the air of preheating are with 50m
3The flow of/h and hydrogen are with 9m
3The flow of/h is from by feeding at the bottom of molecular sieve reaction tower 6 towers that molecular sieve is housed.100 ℃-150 ℃ of control reaction temperature, reaction pressure 0.2-0.5Mpa; Katalysis reaction through catalyzer generates pinacol and a spot of water byproduct; Reaction product is collected from the product scoop 7 of molecular sieve reaction tower 6 bottoms; Pinacol product production 40-42kg/h, the generation 2-3kg/h of water byproduct.
Excessive and reaction does not have completely that butylene, air do not eject the back to get into condensing surface 1 from molecular sieve reaction tower 6, and the butylene of the condensation back of coming out from condensing surface 1 bottom is reclaimed and got into butylene groove 2, unnecessary air emptying.
To react the moisture pinacol of synthetic 1000kg and use the vacuum suction, in moisture pinacol, add Sulfothiorine, until the nondiscoloration of KI starch test paper from product scoop 7.Close the charging opening of rectifying still 15, open hotline heater 13, open rectifying still 15 chuck import and export valves feeding heated oil simultaneously moisture pinacol is heated, be heated to 80-90 ℃, the vacuum valve of opening condensing tower 17 vacuumizes.Temperature is 120-130 ℃ at the bottom of still, 70-80 ℃ of condensation cat head temperature, and cat head begins discharging, puts into scoop 16 and collects.The material of this moment is the higher pinacol of water cut, uses when staying time rectifying.Play stratographic analysis when discharging moisture content reaches 0.2% following time sampling, content was exactly qualified pinacol greater than 99% o'clock at this moment.Put into scoop 16 and collect, use the plastic tank packing.When at the bottom of the still during surplus a spot of material, stop discharging, the still bed material drops into when staying time rectifying again, and rectifying finishes.
Claims (5)
1. one kind is adopted molecular sieve adsorption 2; The method of the synthetic pinacol of 3 dimethyl--2-butylene, it is synthetic, refining that its step comprises, and it is characterized in that: synthesis step is specially: with 2; 3 dimethyl--2-butylene, hydrogen, air feed reaction tower respectively after being heated to 70 ℃-120 ℃ mixes; Make mixture under 100 ℃-150 ℃ temperature, under the reaction pressure of 0.2-0.5Mpa, under the effect of the platinum-palladium-osmium catalyst series of molecular sieve adsorption, react.
2. method according to claim 1; Its characteristic also is: described air heating step is: air is compressed to 0.4-0.8Mpa through air compressor machine; Get into the preheating of air internals preheating in the reaction tower, get into well heater then and heat, with air heating to 70 ℃-120 ℃; Get into the air cushioning jar again and cushion, air pressure is transferred to 0.2-0.5Mpa.
3. method according to claim 1, its characteristic also is: described 2,3 dimethyl--2-butylene heating steps is: with 2; 3 dimethyl--2-butylene, gets into gasification tank again and is heated to 70 ℃-120 ℃ with being pumped into 2, the 3 dimethyl--2-butylene preheating internals preheating in the reaction tower from storage tank; Get into 2 again; 3 dimethyl--2-butylene surge tank cushions, and 2,3 dimethyl--2-butylene pressure is transferred to 0.2-0.5Mpa.
4. method according to claim 1; Its characteristic also is: described hydrogen heating steps is: raw hydrogen is got into the hydrogen preheating internals preheating in the reaction tower from storage tank under the pressure of 0.4-0.8Mpa; Get into heating tank again and be heated to 70 ℃-120 ℃; Get into hydrogen gas buffer again and cushion, hydrogen pressure is transferred to 0.2-0.5Mpa.
5. method according to claim 1 is characterized in that: the molar ratio of material of described mixture is 2,3 dimethyl--2-butylene: hydrogen: air=1.1-1.4:1:6-10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010566944A CN102304020A (en) | 2010-12-01 | 2010-12-01 | Method for synthesizing pinacol by absorbing 2,3-dimethyl-2-butene with molecular sieve |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010566944A CN102304020A (en) | 2010-12-01 | 2010-12-01 | Method for synthesizing pinacol by absorbing 2,3-dimethyl-2-butene with molecular sieve |
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| CN102304020A true CN102304020A (en) | 2012-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201010566944A Pending CN102304020A (en) | 2010-12-01 | 2010-12-01 | Method for synthesizing pinacol by absorbing 2,3-dimethyl-2-butene with molecular sieve |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408397A (en) * | 2013-08-28 | 2013-11-27 | 湖南大乘医药化工有限公司 | Vacuum dewatering-rectifying purifying process of pinacol |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4384146A (en) * | 1979-12-14 | 1983-05-17 | Shell Oil Company | Process for butanediols |
| WO2002088102A1 (en) * | 2001-05-01 | 2002-11-07 | Union Carbide Chemicals & Plastics Technology Corporation | Synthesis of lower alkylene oxides and lower alkylene glycols from lower alkanes and/or lower alkenes |
| CN1622927A (en) * | 2002-01-24 | 2005-06-01 | 独立行政法人产业技术综合研究所 | Novel process for producing 1,2-diol |
| CN101597211A (en) * | 2009-07-09 | 2009-12-09 | 华南理工大学 | A kind of 1, the preparation method of 2-vicinal diol compound |
-
2010
- 2010-12-01 CN CN201010566944A patent/CN102304020A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4384146A (en) * | 1979-12-14 | 1983-05-17 | Shell Oil Company | Process for butanediols |
| WO2002088102A1 (en) * | 2001-05-01 | 2002-11-07 | Union Carbide Chemicals & Plastics Technology Corporation | Synthesis of lower alkylene oxides and lower alkylene glycols from lower alkanes and/or lower alkenes |
| CN1507438A (en) * | 2001-05-01 | 2004-06-23 | ����̼����ѧ�����ϼ�����˾ | Synthesis of lower alkylene oxdies and lower alkylene glycols from lower alkanes and/or lower alkenes |
| CN1622927A (en) * | 2002-01-24 | 2005-06-01 | 独立行政法人产业技术综合研究所 | Novel process for producing 1,2-diol |
| CN101597211A (en) * | 2009-07-09 | 2009-12-09 | 华南理工大学 | A kind of 1, the preparation method of 2-vicinal diol compound |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408397A (en) * | 2013-08-28 | 2013-11-27 | 湖南大乘医药化工有限公司 | Vacuum dewatering-rectifying purifying process of pinacol |
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Application publication date: 20120104 |