CN106040265A - Method for preparing catalyst for synthesizing methyl tert-butyl ether - Google Patents
Method for preparing catalyst for synthesizing methyl tert-butyl ether Download PDFInfo
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- C07C41/09—Preparation of ethers by dehydration of compounds containing hydroxy groups
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Abstract
The invention relates to a method for preparing a catalyst for synthesizing methyl tert-butyl ether and belongs to the technical field of methyl tert-butyl ether (MTBE) preparation. The method comprises a first step of preparing precursor powder; a second step of preparing a catalyst carrier; a third step of soaking the catalyst carrier in a sulfuric acid solution with a concentration of 2 mol/L based on the requirement that the weight of the sulfuric acid solution is 0.5-1 times that of the catalyst carrier, taking out the catalyst carrier, performing natural drying, and performing roasting for 4-5 h at 400-500 DEG C to obtain the catalyst. A method for further synthesizing methyl tert-butyl ether under the effect of the catalyst by using tert-butyl alcohol and methanol is provided, and the method has the advantage of being high in conversion rate.
Description
Technical field
The present invention relates to the preparation method of a kind of methyl tertiary butyl ether(MTBE) catalyst for synthesizing, belong to MTBE technology of preparing neck
Territory.
Background technology
Methyl tertiary butyl ether(MTBE) (MTBE) has excellent performance as gasoline additive, not only has the highest clean octane
Value, and have good for various gasoline such as direct steaming gasoline, gasoline alkylate, catalytically cracked gasoline, catalytic reforming gasoline
Mediation effect, has higher mediation octane number.Entering a small amount of MTBE in the oil just can make octane number have bigger increasing
Add.
The production technology of MTBE continuously improves also with continuing to increase of Production requirement, by the beginning of the 70's with moral
State's HULS technique is the employing shell and tube reactor of representative, and shell side walks cooling water process；Develop into adopting of later stage in the 70's
With cartridge reactor, outer circulation heating picking process；Entering for the 80's, reactor is merged by catalytic distillation technology with product fractional distillation.
1st set catalytic distillation process produces the commercial plant of MTBE and built in Houston oil plant in 1981；By 90 years
In generation, butane isomerization dehydrogenation generates the process integration of MTBE with methanol etherification.MTBE process units is substantially all and adopts now
The technique taking isobutene. and methanol-fueled CLC.
CN102351661A discloses a kind of method preparing methyl tertiary butyl ether(MTBE), at original mixed phase fixed bed reactors
One outer circulation of front concatenation takes thermosetting fixed bed reactor, comprises the following steps that and first raw material mixing C4 input outer circulation is taken heat
Fixed bed reactors carry out react the isobutene content so that in raw material mixing C4 and is reduced to below 30 weight %；Again will reaction
After material enter in mixed phase fixed bed reactors and react；Enter from mixed phase fixed bed reactors reaction mass out and urge
Change distillation column carry out degree of depth etherificate and separate.CN105218325A discloses the preparation work of a kind of low-sulfur methyl tertiary butyl ether(MTBE)
Skill, this technique is by by the liquefied petroleum gas C 4 fraction after agent alkali desulphurization alcohol and methanol mixed, is introduced into methyltertiarvbutyl ether reactor
Carry out catalytic reaction, enter back into catalytic reaction-separated tower and carry out catalytic reaction, catalytic reaction gained sulfur compound further
MTBE mix products from the bottom of catalytic reaction-separated tower tower out, sequentially pass through lightness-removing column removing less than MTBE proportion
Trechmannite compound, removes more heavy heavy sulfide than MTBE through weight-removing column, obtains low-sulfur MTBE product.
But above-mentioned method is suitable catalyst owing to catalytic reaction lacks, also exist synthetic method yield low, select
Property difference problem.
Summary of the invention
It is an object of the invention to: a kind of catalyst for synthesizing is provided, and utilize the tert-butyl alcohol and methanol as raw material, at this
The method of next step synthesizing methyl tertbutyl ether of catalyst action, the method has the advantage that conversion ratio is high.
Technical scheme is:
First provide the preparation method of methyl tertiary butyl ether(MTBE) catalyst for synthesizing, comprise the steps:
1st step, by weight, by 140～180 parts of Ni (NO3)2·6H2O, 10～30 parts of La (NO3)3·6H2O is dissolved in
In 500～800 parts of deionized waters and stir formation the first solution；By 50～120 parts of Mn (NO3)2, 15～20 parts of Zr
(NO3)2·5H2O is dissolved in 100～300 parts of deionized waters and stirs and forms the second solution；Under agitation by 150
～200 parts of Al2O3It is uniform that powder is slowly added to the first solution & stir, then is added thereto to the second solution successively, after stirring,
Add the Na of 20wt% concentration2CO3Solution makes precipitation by metallic ion, and the precipitate after washing, drying enters under the conditions of 120 DEG C
Row is dried 8 hours, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 20～30 parts, five n-butoxy niobiums 5～10 parts, zirconium-n-propylate 40～50
Part, isopropanol 200～300 parts, mix homogeneously, obtain mixed solution；Then take 10～20wt% salpeter solutions 70～80 parts, drip
Add in mixed solution, stir, make reaction 2～4 hours, to let cool to room temperature, take off the milky white liquid of layer, adjust with 20wt% ammonia
Joint pH to 8～10, add Precursor Powder 10～30 parts stir, then be warming up to 70～90 DEG C react 6～8 hours, let cool
After, it is aged 12～24 days at 20～30 DEG C；The ageing liquid of gained is filtered, roasting will be carried out at powder body 700～800 DEG C
After 3～4 hours, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
0.5～1 times, after taking-up, naturally dry, then carry out at 400～500 DEG C roasting 4～after 5 hours, obtain catalyst.
Next provides the method applying above-mentioned catalyst synthesizing methyl tertbutyl ether, comprises the steps:
1st step, gasifies the mixed liquor of the tert-butyl alcohol and methanol, sends into and urges equipped with in the fixed bed reactors of catalyst
Change reaction, reaction generate gas phase condensed after, obtain condensed fluid；
2nd step, distills condensed fluid, the fraction between collecting 40～60 DEG C, washes after being condensed by this fraction, will divide
The ether layer gone out adds water absorbing agent, after removing moisture, then leaches water absorbing agent, distill again after ether layer adds metallic sodium,
Fraction between collecting 54～56 DEG C, obtains product methyl tertiary butyl ether(MTBE).
In the 1st described step, the raw materials components mole ratio scope of the tert-butyl alcohol and methanol is 1:2～4, reaction temperature 110～120
℃。
In the 1st described step, the catalytic reaction space velocity range of reacting gas is 0.90～1.00ml/g h.
In the 2nd described step, water absorbing agent is natrium carbonicum calcinatum.
In the 2nd described step, in order to remove the water in ether layer further, after leaching water absorbing agent, in addition it is also necessary in ether layer
Middle addition metallic sodium.
Beneficial effect
What the present invention provided utilizes the tert-butyl alcohol and methanol as raw material at next step synthesizing methyl tertbutyl ether of catalyst action
Method, the method has the advantage that conversion ratio is high.
Detailed description of the invention
Embodiment 1
1st step, gasifies the mixed liquor of the tert-butyl alcohol and methanol, sends into and urges equipped with in the fixed bed reactors of catalyst
Changing reaction, the raw materials components mole ratio scope of the tert-butyl alcohol and methanol is 1:2, reaction temperature 110 DEG C, the catalytic reaction air speed of reacting gas
Scope is 0.90ml/g h, reaction generate gas phase condensed after, obtain condensed fluid；
2nd step, distills condensed fluid, the fraction between collecting 40～60 DEG C, washes after being condensed by this fraction, will divide
The ether layer gone out adds natrium carbonicum calcinatum water absorbing agent, after removing moisture, then leaches water absorbing agent, in ether layer after addition metallic sodium again
Distill, the fraction between collecting 54～56 DEG C, obtain product methyl tertiary butyl ether(MTBE).
In the 1st described step, the preparation method of described catalyst is as follows:
1st step, by weight, by 140 parts of Ni (NO3)2·6H2O, 10 parts of La (NO3)3·6H2O be dissolved in 500 parts go from
In sub-water and stir formation the first solution；By 50 parts of Mn (NO3)2, 15 parts of Zr (NO3)2·5H2O is dissolved in 100 parts of deionizations
In water and stir formation the second solution；Under agitation by 150 parts of Al2O3It is equal that powder is slowly added to the first solution & stir
Even, then it is added thereto to the second solution successively, after stirring, add the Na of 20wt% concentration2CO3Solution makes metal ion sink
Forming sediment, the precipitate after washing, drying carries out drying 8 hours under the conditions of 120 DEG C, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 20 parts, five n-butoxy niobium 5 parts, zirconium-n-propylate 40 parts, isopropanol 200
Part, mix homogeneously, obtain mixed solution；Then take 10wt% salpeter solution 70 parts, drip in mixed solution, stir, make
React 2 hours, let cool to room temperature, take off the milky white liquid of layer, regulate pH to 8 with 20wt% ammonia, add Precursor Powder 10 parts stirring
Uniformly, then it is warming up to 70 DEG C of reactions 6 hours, after letting cool, is aged 12 days at 20 DEG C；The ageing liquid of gained is filtered, will
After carrying out roasting 3 hours at powder body 700 DEG C, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
0.5 times, after taking-up, naturally dry, then after carrying out at 400 DEG C roasting 4 hours, obtain catalyst.
Embodiment 2
1st step, gasifies the mixed liquor of the tert-butyl alcohol and methanol, sends into and urges equipped with in the fixed bed reactors of catalyst
Changing reaction, the raw materials components mole ratio scope of the tert-butyl alcohol and methanol is 1:4, reaction temperature 120 DEG C, and the catalytic reaction of reacting gas is empty
Speed scope be 1.00ml/g h, reaction generate gas phase condensed after, obtain condensed fluid；
2nd step, distills condensed fluid, the fraction between collecting 40～60 DEG C, washes after being condensed by this fraction, will divide
The ether layer gone out adds natrium carbonicum calcinatum water absorbing agent, after removing moisture, then leaches water absorbing agent, in ether layer after addition metallic sodium again
Distill, the fraction between collecting 54～56 DEG C, obtain product methyl tertiary butyl ether(MTBE).
In the 1st described step, the preparation method of described catalyst is as follows:
1st step, by weight, by 180 parts of Ni (NO3)2·6H2O, 30 parts of La (NO3)3·6H2O is dissolved in 800 parts of deionizations
In water and stir formation the first solution；By 120 parts of Mn (NO3)2, 20 parts of Zr (NO3)2·5H2O is dissolved in 300 parts of deionizations
In water and stir formation the second solution；Under agitation by 200 parts of Al2O3It is equal that powder is slowly added to the first solution & stir
Even, then it is added thereto to the second solution successively, after stirring, add the Na of 20wt% concentration2CO3Solution makes metal ion sink
Forming sediment, the precipitate after washing, drying carries out drying 8 hours under the conditions of 120 DEG C, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 30 parts, five n-butoxy niobium 10 parts, zirconium-n-propylate 50 parts, isopropanol 300
Part, mix homogeneously, obtain mixed solution；Then take 20wt% salpeter solution 80 parts, drip in mixed solution, stir, make
React 4 hours, let cool to room temperature, take off the milky white liquid of layer, regulate pH to 10 with 20wt% ammonia, add Precursor Powder 30 parts and stir
Mix uniformly, then be warming up to 90 DEG C of reactions 8 hours, after letting cool, be aged 24 days at 30 DEG C；The ageing liquid of gained is filtered,
Roasting 3 will be carried out at powder body 800 DEG C～after 4 hours, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
1 times, after taking-up, naturally dry, then after carrying out at 500 DEG C roasting 5 hours, obtain catalyst.
Embodiment 3
1st step, gasifies the mixed liquor of the tert-butyl alcohol and methanol, sends into and urges equipped with in the fixed bed reactors of catalyst
Changing reaction, the raw materials components mole ratio scope of the tert-butyl alcohol and methanol is 1:3, reaction temperature 115 DEG C, the catalytic reaction air speed of reacting gas
Scope is 0.95ml/g h, reaction generate gas phase condensed after, obtain condensed fluid；
2nd step, distills condensed fluid, the fraction between collecting 40～60 DEG C, washes after being condensed by this fraction, will divide
The ether layer gone out adds natrium carbonicum calcinatum water absorbing agent, after removing moisture, then leaches water absorbing agent, in ether layer after addition metallic sodium again
Distill, the fraction between collecting 54～56 DEG C, obtain product methyl tertiary butyl ether(MTBE).
In the 1st described step, the preparation method of described catalyst is as follows:
1st step, by weight, by 160 parts of Ni (NO3)2·6H2O, 18 parts of La (NO3)3·6H2O be dissolved in 600 parts go from
In sub-water and stir formation the first solution；By 70 parts of Mn (NO3)2, 18 parts of Zr (NO3)2·5H2O is dissolved in 190 parts of deionizations
In water and stir formation the second solution；Under agitation by 160 parts of Al2O3It is equal that powder is slowly added to the first solution & stir
Even, then it is added thereto to the second solution successively, after stirring, add the Na of 20wt% concentration2CO3Solution makes metal ion sink
Forming sediment, the precipitate after washing, drying carries out drying 8 hours under the conditions of 120 DEG C, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 26 parts, five n-butoxy niobium 6 parts, zirconium-n-propylate 46 parts, isopropanol 240
Part, mix homogeneously, obtain mixed solution；Then take 17wt% salpeter solution 76 parts, drip in mixed solution, stir, make
React 3 hours, let cool to room temperature, take off the milky white liquid of layer, regulate pH to 9 with 20wt% ammonia, add Precursor Powder 18 parts stirring
Uniformly, then it is warming up to 78 DEG C of reactions 7 hours, after letting cool, is aged 20 days at 24 DEG C；The ageing liquid of gained is filtered, will
After carrying out roasting 4 hours at powder body 750 DEG C, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
0.8 times, after taking-up, naturally dry, then after carrying out at 450 DEG C roasting 4 hours, obtain catalyst.
Reference examples 1
Difference with embodiment 3 is: do not add La (NO in the 1st step in the preparation process of catalyst3)3·6H2O。
1st step, gasifies the mixed liquor of the tert-butyl alcohol and methanol, sends into enter equipped with in the fixed bed reactors of catalyst
The raw materials components mole ratio scope of row catalytic reaction, the tert-butyl alcohol and methanol is 1:3, reaction temperature 115 DEG C, the catalytic reaction of reacting gas
Space velocity range is 0.95ml/g h, reaction generate gas phase condensed after, obtain condensed fluid；
2nd step, distills condensed fluid, the fraction between collecting 40～60 DEG C, washes after being condensed by this fraction, will divide
The ether layer gone out adds natrium carbonicum calcinatum water absorbing agent, after removing moisture, then leaches water absorbing agent, in ether layer after addition metallic sodium again
Distill, the fraction between collecting 54～56 DEG C, obtain product methyl tertiary butyl ether(MTBE).
In the 1st described step, the preparation method of described catalyst is as follows:
1st step, by weight, by 160 parts of Ni (NO3)2·6H2O is dissolved in 600 parts of deionized waters and stirs formation
First solution；By 70 parts of Mn (NO3)2, 18 parts of Zr (NO3)2·5H2O is dissolved in 190 parts of deionized waters and stirs formation
Two solution；Under agitation by 160 parts of Al2O3It is uniform that powder is slowly added to the first solution & stir, then is added thereto to the successively
Two solution, after stirring, add the Na of 20wt% concentration2CO3Solution makes precipitation by metallic ion, sinking after washing, drying
Shallow lake thing carries out drying 8 hours under the conditions of 120 DEG C, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 26 parts, five n-butoxy niobium 6 parts, zirconium-n-propylate 46 parts, isopropanol 240
Part, mix homogeneously, obtain mixed solution；Then take 17wt% salpeter solution 76 parts, drip in mixed solution, stir, make
React 3 hours, let cool to room temperature, take off the milky white liquid of layer, regulate pH to 9 with 20wt% ammonia, add Precursor Powder 18 parts stirring
Uniformly, then it is warming up to 78 DEG C of reactions 7 hours, after letting cool, is aged 20 days at 24 DEG C；The ageing liquid of gained is filtered, will
After carrying out roasting 4 hours at powder body 750 DEG C, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
0.8 times, after taking-up, naturally dry, then after carrying out at 450 DEG C roasting 4 hours, obtain catalyst.
Reference examples 2
Difference with embodiment 3 is: do not add Zr (NO in the 1st step in the preparation process of catalyst3)2·5H2O。
1st step, gasifies the mixed liquor of the tert-butyl alcohol and methanol, sends into enter equipped with in the fixed bed reactors of catalyst
The raw materials components mole ratio scope of row catalytic reaction, the tert-butyl alcohol and methanol is 1:3, reaction temperature 115 DEG C, the catalytic reaction of reacting gas
Space velocity range is 0.95ml/g h, reaction generate gas phase condensed after, obtain condensed fluid；
2nd step, distills condensed fluid, the fraction between collecting 40～60 DEG C, washes after being condensed by this fraction, will divide
The ether layer gone out adds natrium carbonicum calcinatum water absorbing agent, after removing moisture, then leaches water absorbing agent, in ether layer after addition metallic sodium again
Distill, the fraction between collecting 54～56 DEG C, obtain product methyl tertiary butyl ether(MTBE).
In the 1st described step, the preparation method of described catalyst is as follows:
1st step, by weight, by 160 parts of Ni (NO3)2·6H2O, 18 parts of La (NO3)3·6H2O be dissolved in 600 parts go from
In sub-water and stir formation the first solution；By 70 parts of Mn (NO3)2Be dissolved in 190 parts of deionized waters and stir formation
Second solution；Under agitation by 160 parts of Al2O3It is uniform that powder is slowly added to the first solution & stir, then is added thereto to successively
Second solution, after stirring, adds the Na of 20wt% concentration2CO3Solution makes precipitation by metallic ion, after washing, drying
Precipitate carries out drying 8 hours under the conditions of 120 DEG C, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 26 parts, five n-butoxy niobium 6 parts, zirconium-n-propylate 46 parts, isopropanol 240
Part, mix homogeneously, obtain mixed solution；Then take 17wt% salpeter solution 76 parts, drip in mixed solution, stir, make
React 3 hours, let cool to room temperature, take off the milky white liquid of layer, regulate pH to 9 with 20wt% ammonia, add Precursor Powder 18 parts stirring
Uniformly, then it is warming up to 78 DEG C of reactions 7 hours, after letting cool, is aged 20 days at 24 DEG C；The ageing liquid of gained is filtered, will
After carrying out roasting 4 hours at powder body 750 DEG C, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
0.8 times, after taking-up, naturally dry, then after carrying out at 450 DEG C roasting 4 hours, obtain catalyst.
| MTBE Synthesis conversion % | MTBE synthesis of selective % | |
| Embodiment 1 | 46.4 | 81.4 |
| Embodiment 2 | 47.3 | 83.2 |
| Embodiment 3 | 49.5 | 85.0 |
| Reference examples 1 | 45.2 | 77.5 |
| Reference examples 2 | 44.9 | 76.8 |
As can be seen from the table, the conversion ratio of the MTBE synthetic method that the present invention provides is more than 45%, and embodiment 3 is relative to right
As usual for 1, the preparation of catalyst adds La, improves Synthesis conversion；Embodiment 3 for reference examples 2,
In the preparation of catalyst, add Zr, improve synthesis of selective.
Claims (1)
1. the preparation method of a methyl tertiary butyl ether(MTBE) catalyst for synthesizing, it is characterised in that comprise the steps:
1st step, by weight, by 140～180 parts of Ni (NO3)2·6H2O, 10～30 parts of La (NO3)3·6H2O is dissolved in
In 500～800 parts of deionized waters and stir formation the first solution；By 50～120 parts of Mn (NO3)2, 15～20 parts of Zr
(NO3)2·5H2O is dissolved in 100～300 parts of deionized waters and stirs and forms the second solution；Under agitation by 150
～200 parts of Al2O3It is uniform that powder is slowly added to the first solution & stir, then is added thereto to the second solution successively, after stirring,
Add the Na of 20wt% concentration2CO3Solution makes precipitation by metallic ion, and the precipitate after washing, drying enters under the conditions of 120 DEG C
Row is dried 8 hours, obtains Precursor Powder；
2nd step, by weight, takes butyl titanate 20～30 parts, five n-butoxy niobiums 5～10 parts, zirconium-n-propylate 40～50
Part, isopropanol 200～300 parts, mix homogeneously, obtain mixed solution；Then take 10～20wt% salpeter solutions 70～80 parts, drip
Add in mixed solution, stir, make reaction 2～4 hours, to let cool to room temperature, take off the milky white liquid of layer, adjust with 20wt% ammonia
Joint pH to 8～10, add Precursor Powder 10～30 parts stir, then be warming up to 70～90 DEG C react 6～8 hours, let cool
After, it is aged 12～24 days at 20～30 DEG C；The ageing liquid of gained is filtered, roasting will be carried out at powder body 700～800 DEG C
After 3～4 hours, prepare catalyst carrier；
3rd step, is placed in 2mol/L sulfuric acid solution immersion by catalyst carrier, and the weight of sulfuric acid solution is catalyst carrier weight
0.5～1 times, after taking-up, naturally dry, then carry out at 400～500 DEG C roasting 4～after 5 hours, obtain catalyst.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109232196A (en) * | 2018-10-30 | 2019-01-18 | 安徽海德化工科技有限公司 | A kind of preparation method of methyl tertiary butyl ether(MTBE) |
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| CN109232196A (en) * | 2018-10-30 | 2019-01-18 | 安徽海德化工科技有限公司 | A kind of preparation method of methyl tertiary butyl ether(MTBE) |
| CN109232196B (en) * | 2018-10-30 | 2021-06-08 | 蚌埠知博自动化技术开发有限公司 | Preparation method of methyl tert-butyl ether |
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