CN103571532A - Pre-etherification reaction method in light petrol etherification technology - Google Patents
Pre-etherification reaction method in light petrol etherification technology Download PDFInfo
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Abstract
The invention provides a pre-etherification reaction method in a light petrol etherification technology, which comprises the steps that light petrol, methanol and a catalyst are added into an external membrane reactor comprising a reaction kettle and a ceramic membrane filter at a weight ratio of 1:(0.01-0.1):(1-20); the catalyst is a fine-grained styrene cation exchange resin catalyst; the light petrol and methanol perform continuous catalytic etherification reaction in the reaction kettle; a reaction mixture is pumped to the ceramic membrane filter from the bottom of the reaction kettle for catalyst and reaction product separation; a separated product penetrates from a membrane tube as clear liquid; the flow of the membrane penetrating liquid is controlled to be the same as the total amount of a reactant entering the reaction kettle; the reaction product performs further etherification reaction; concentrated liquid containing the catalyst returns to the reaction kettle. Since the method employs the external membrane reactor and the fine-grained resin catalyst, a catalytic effect is significantly improved.
Description
Technical field
The present invention relates to a kind of deolefination method in petroleum naphtha, particularly a kind of method of pre-etherification reaction in Etherification of Light FCC Gasoline technique.
Background technology
Etherification of Light FCC Gasoline technology utilizes tertiary amylene and the tertiary hexene in catalytically cracked gasoline to react ether compounds such as generating TAME, THXME with methyl alcohol, can improve gasoline octane rating, reduces olefin(e) centent and vapour pressure.Etherification of Light FCC Gasoline be mainly can etherificate hydrocarbon fraction in gasoline under an acidic catalyst condition, with the etherification reaction of methyl alcohol, and be mainly C
5, C
6can etherificate alkene etherification reaction, generate corresponding ether product, wherein 2-methyl butene-1 and the reaction of 2-methyl butene-2 are as follows:
BP oil company etherification technology adopts the three function catalyzer that have hydrogenation, isomery and etherificate concurrently, take that to be less than the catalytic light gasoline of 77 ℃ be raw material, in German Vohburg refinery, build up Etherification of Light FCC Gasoline device, form BP oil company light FCC gasoline etherification technology technology.
Finland Neste company Etherification of Light FCC Gasoline technology is the noble metal catalyst that adopts inorganic carrier load, as diolefine selective hydrogenation catalyst in petroleum naphtha, the petroleum naphtha containing C4～C7 cut of processing through selective hydrogenation and methyl alcohol are sent into pre-reactor and are carried out etherification reaction, etherification reaction product is sent to distillation tower fractionation, and ether compound and high-boiling hydrocarbons are discharged from the bottom of tower.
The Etherification of Light FCC Gasoline technique of Mobil company is that excessive lower alcohol and petroleum naphtha are mixed, and first carries out etherificate for the first time, then carries out fractionation, contains the following hydro carbons of methyl alcohol and C5 in lighting end, contains the above hydro carbons of ether and C5 in last running, and etherificate is carried out in lighting end again.Etherificate adopts an acidic catalyst for the first time, and etherificate adopts metal silicate catalysts for the second time.Thereby the olefin(e) centent in reduction gasoline, improves gasoline octane rating.
In order to reduce investment outlay and to improve reaction efficiency, as the catalytic distillation tower of Etherification of Light FCC Gasoline device is last, establish 1 pre-reactor, in gasoline, can in pre-reactor, after preliminary conversion, enter in catalytic distillation tower again and continue reaction by etherificate alkene, the form of pre-reactor has mixed phase fixed bed, outer circulation fixed bed etc. according to the difference of iso-butylene content in raw material.
It is large that above patent system Preparation Method all has resin catalyst consumption, the shortcoming that etherification reaction transformation efficiency is lower.
The appearance of membrane reactor technology, has realized the coupling of membrane separation technique and reaction process, has solved that its flow process is long, inefficiency, problem that energy consumption is higher.Associating Nanjing JiuSi High-Tech Co.,Ltd of Nanjing University of Technology, by to the scientific research of two more than ten years of continuous ceramic membrane reactor, successfully develop the ceramic membrane product of plurality of specifications and model, having realized membrane reactor produces in large-scale application and the serialization of petrochemical field, ceramic membrane reactor can significantly shorten chemical industry Production Flow Chart, improves product yield, reduce production costs, reduces " three wastes " discharge, has resources conservation, eco-friendly feature.
Summary of the invention
Based on above-mentioned background technology, the object of the invention is to, for the deficiencies in the prior art, provide the method for pre-etherification reaction in a kind of Etherification of Light FCC Gasoline technique, effectively solve the recycle problem of catalyzer, shortened process, realizes the serialization of production process.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
Before entering catalytic distillation tower, use petroleum naphtha and methyl alcohol as raw material, in external placed type membrane reactor, carry out the pre-etherification reaction of continuous catalysis, catalyzer adopts fine particle styrene type cation exchange resin catalyzer, form reaction and separation coupling system, the recycle problem that has effectively solved thus catalyzer, has shortened technical process, has realized the serialization of production process.
Technical scheme of the present invention specifically comprises:
By petroleum naphtha, methyl alcohol adds the external membrane reactor that comprises reactor and purpose ceramic-film filter with catalyzer together with the weight ratio of 1:0.01～0.1:1～20, described catalyzer is fine particle styrene type cation exchange resin catalyzer, petroleum naphtha carries out continuous catalyst etherifying and reacts in described reactor with methyl alcohol, reaction mixture is pumped into purpose ceramic-film filter separating catalyst and reaction product from reactor bottom, isolated product oozes out from film pipe in the mode of clear liquid, membrane permeation flow quantity is automatically controlled consistent with the total amount of reactant that enters reactor, reaction product is sent into the further etherification reaction of catalytic rectifying tower, and the dope that contains catalyzer returns to reactor.Described fine particle styrene type cation exchange resin catalyzer can be selected commercially available prod, as D006 resin catalyst, the KC116 resin catalyst that Kairui Chemical Co., Ltd. produces, the A35 resin catalyst that D006-7 small particle size resin catalyst or U.S. Rhom and Hass produce; The short grained resin catalyst of preferable particle size 70-120 order; More preferably the short grained resin catalyst of particle diameter 70-100 order.
Described external membrane reactor can be selected the XS-T type external membrane reactor of commercially available prod ，Ru Nanjing University of Technology and Nanjing JiuSi High-Tech Co.,Ltd's joint production.
When described raw material enters reactor, the weight ratio of petroleum naphtha, methyl alcohol and catalyzer is preferably 1:0.1:5.。
In described continuous catalysis etherification reaction, 60～100 ℃ of preferable reaction temperature, air speed 0.5～3/h, reaction pressure 0.4～1MPa.
A preferred embodiment of the present invention comprises the following steps:
By petroleum naphtha, methyl alcohol adds the external membrane reactor that comprises reactor and purpose ceramic-film filter with catalyzer together with the weight ratio of 1:0.1:5, described catalyzer is particle diameter 70-100 object fine particle styrene type cation exchange resin catalyzer, petroleum naphtha carries out continuous catalyst etherifying and reacts in described reactor with methyl alcohol, 60～100 ℃ of temperature of reaction, air speed 0.5～3/h, reaction pressure 0.4～1MPa, reaction mixture is pumped into purpose ceramic-film filter separating catalyst and reaction product from reactor bottom, isolated product oozes out from film pipe in the mode of clear liquid, membrane permeation flow quantity is automatically controlled consistent with the total amount of reactant that enters reactor, reaction product is sent into the further etherification reaction of catalytic rectifying tower, and the dope that contains catalyzer returns to reactor.
The present invention has following beneficial effect:
In the inventive method, adopt external membrane reactor for adopting short grained resin catalyst to create condition, small-particle resin catalyst specific surface area is large, and unit volume amounts of particles is many, and the sulfonic group content of unit volume is high, and catalytic effect is improved.And catalyst particle is used in fixed bed, can cause bed resistance large, impact is produced and is normally carried out, and in membrane reactor, resin, in flow state, fully contacts with reactant, has improved reaction efficiency, has overcome the shortcoming of fixed bed.
Embodiment
Following instance is only to further illustrate the present invention, is not restriction the scope of protection of the invention.
Embodiment 1:
Equipment: XS-T type external membrane reactor 10L， Nanjing University of Technology produces, and structure comprises reactor and purpose ceramic-film filter.
Technical process: petroleum naphtha, methyl alcohol and catalyzer are added to above-mentioned external membrane reactor according to the weight ratio of 1:0.1:5, and petroleum naphtha mixes after reaction mass preheating with methyl alcohol is carried out continuous etherification reaction with the mol ratio of setting in reactor.The short grained D006-7 resin catalyst of particle diameter 70-100 order that catalyzer adopts 2L Kairui Chemical Co., Ltd. to produce, the moisture in catalyzer is replaced to water content≤1% with methyl alcohol, 80 ℃ of temperature of reaction, air speed 1h
-1alcohol oil quality is than 0.01, reaction pressure 0.4MPa, reaction mixture is pumped into purpose ceramic-film filter from reactor bottom, under certain pressure reduction promotes, realize the separated of catalyzer and reaction product, wherein product oozes out from film pipe in the mode of clear liquid, and membrane permeation flow quantity is controlled consistent with the total amount of reactant that enters reactor automatically.Pre-etherification reaction product is sent into the further etherification reaction of catalytic rectifying tower, and the dope that contains catalyzer returns to reactor.Pre-etherificate products obtained therefrom is numbered KRB-1.
Embodiment 2
90 ℃ of temperature of reaction, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-2.
Embodiment 3
Air speed 3h
-1, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-3.
Embodiment 4
Air speed 3h
-1, the other the same as in Example 2.Pre-etherificate products obtained therefrom is numbered KRB-4.
Embodiment 5
Air speed 0.5h
-1, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-5.
Embodiment 6
Alcohol oil quality is than 0.05, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-6.
Embodiment 7
Alcohol oil quality is than 0.05, the other the same as in Example 2.Pre-etherificate products obtained therefrom is numbered KRB-7.
Embodiment 8
Alcohol oil quality is than 0.05, the other the same as in Example 3.Pre-etherificate products obtained therefrom is numbered KRB-8.
Embodiment 9
Alcohol oil quality is than 0.05, the other the same as in Example 4.Pre-etherificate products obtained therefrom is numbered KRB-9.
Embodiment 10.
Alcohol oil quality is than 0.05, the other the same as in Example 5.Pre-etherificate products obtained therefrom is numbered KRB-10.
Embodiment 11.
Alcohol oil quality is than 0.05, and other is with embodiment 6.Pre-etherificate products obtained therefrom is numbered KRB-11.
Embodiment 12.
Reaction pressure 1MPa, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-12.
Embodiment 13.
Reaction pressure 1MPa, the other the same as in Example 2.Pre-etherificate products obtained therefrom is numbered KRB-13.
Embodiment 14.
Reaction pressure 1MPa, the other the same as in Example 3.Pre-etherificate products obtained therefrom is numbered KRB-14.
Embodiment 15.
Reaction pressure 1MPa, the other the same as in Example 4.Pre-etherificate products obtained therefrom is numbered KRB-15.
Embodiment 16.
Reaction pressure 1MPa, the other the same as in Example 5.Pre-etherificate products obtained therefrom is numbered KRB-16.
Embodiment 17.
Reaction pressure 1MPa, other is with embodiment 6.Pre-etherificate products obtained therefrom is numbered KRB-17.
Embodiment 18.
Alcohol oil quality is than 0.1, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-18.
Embodiment 19
60 ℃ of temperature of reaction, the other the same as in Example 1.Pre-etherificate products obtained therefrom is numbered KRB-19.
Comparative example 1
Experimental installation is continuous 10L micro fixed-bed reactor, and the long 4000mm of stainless steel tubular type reactor, internal diameter 100mm fill in the D006 granules of catalyst of 4L at the middle part of reactor, 80 ℃ of temperature of reaction, air speed 1h
-1, alcohol oil quality is than 0.01, reaction pressure 1MPa, and pre-etherification reaction product is sent into the further etherification reaction of catalytic rectifying tower, and pre-etherificate products obtained therefrom is numbered KRB-20.
By the pre-etherification reaction 100h of above embodiment, sampling detection reaction raw material and product are analyzed with gas chromatograph.
Table 1: the comparison of the total tertiary carbon olefin conversion of test sample that different process is made.
| Numbering | Total tertiary carbon olefin conversion % |
| KRB－1 | 50 |
| KRB－2 | 52 |
| KRB－3 | 53 |
| KRB－4 | 56 |
| KRB－5 | 63 |
| KRB－6 | 60 |
| KRB－7 | 64 |
| KRB－8 | 62 |
| KRB－9 | 66 |
| KRB－10 | 65 |
| KRB－11 | 60 |
| KRB－12 | 58 |
| KRB－13 | 59 |
| KRB－14 | 61 |
| KRB－15 | 57 |
| KRB－16 | 53 |
| KRB－17 | 74 |
| KRB－18 | 68 |
| KRB－19 | 63 |
| KRB－20 | 55 |
As shown in Table 1: relative fixed bed pre-reaction technique, the method of pre-etherification reaction in Etherification of Light FCC Gasoline technique of the present invention, the external membrane using reacts the catalyzer that pre-etherification technology is only used 0.5 times of quality of fixed-bed process, obtains close or higher total tertiary carbon olefin conversion.Small-particle resin catalyst specific surface area is large, and unit volume amounts of particles is many, and the sulfonic group content of unit volume is high, and catalytic effect is improved.In membrane reactor, resin, in flow state, fully contacts with reactant, has overcome the shortcoming of fixed bed.
Claims (9)
1. the method for pre-etherification reaction in an Etherification of Light FCC Gasoline technique, it is characterized in that, comprise the following steps: by petroleum naphtha, methyl alcohol adds the external membrane reactor that comprises reactor and purpose ceramic-film filter with catalyzer together with the weight ratio of 1:0.01～0.1:1～20, described catalyzer is fine particle styrene type cation exchange resin catalyzer, petroleum naphtha carries out continuous catalyst etherifying and reacts in described reactor with methyl alcohol, reaction mixture is pumped into purpose ceramic-film filter separating catalyst and reaction product from reactor bottom, isolated product oozes out from film pipe in the mode of clear liquid, membrane permeation flow quantity is automatically controlled consistent with the total amount of reactant that enters reactor, reaction product is sent into the further etherification reaction of catalytic rectifying tower, and the dope that contains catalyzer returns to reactor.
2. method claimed in claim 1, it is characterized in that: described fine particle styrene type cation exchange resin catalyzer is selected from D006 resin catalyst, the KC116 resin catalyst that Kairui Chemical Co., Ltd. produces the A35 resin catalyst that D006-7 small particle size resin catalyst or U.S. Rhom and Hass produce.
3. method claimed in claim 1, is characterized in that: described fine particle styrene type cation exchange resin catalyzer is particle diameter 70-120 object small-particle resin catalyst.
4. method claimed in claim 1, is characterized in that: described fine particle styrene type cation exchange resin catalyzer is particle diameter 70-100 object small-particle resin catalyst.
5. method claimed in claim 1, is characterized in that: the weight ratio of described petroleum naphtha, methyl alcohol and catalyzer is 1:0.1:5.
6. method claimed in claim 1, is characterized in that: described continuous catalysis etherification reaction temperature is 60～100 ℃.
7. method claimed in claim 1, is characterized in that: described continuous catalysis etherification reaction air speed is 0.5～3/h.
8. method claimed in claim 1, is characterized in that: described continuous catalysis etherification reaction pressure is 0.4～1MPa.
9. method claimed in claim 1, is characterized in that, step is as follows:
By petroleum naphtha, methyl alcohol adds the external membrane reactor that comprises reactor and purpose ceramic-film filter with catalyzer together with the weight ratio of 1:0.1:5, described catalyzer is particle diameter 70-100 object fine particle styrene type cation exchange resin catalyzer, petroleum naphtha carries out continuous catalyst etherifying and reacts in described reactor with methyl alcohol, 60～100 ℃ of temperature of reaction, air speed 0.5～3/h, reaction pressure 0.4～1MPa, reaction mixture is pumped into purpose ceramic-film filter separating catalyst and reaction product from reactor bottom, isolated product oozes out from film pipe in the mode of clear liquid, membrane permeation flow quantity is automatically controlled consistent with the total amount of reactant that enters reactor, reaction product is sent into the further etherification reaction of catalytic rectifying tower, and the dope that contains catalyzer returns to reactor.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112724000A (en) * | 2019-10-14 | 2021-04-30 | 中国石油化工股份有限公司 | Production method of polymethoxy dimethyl ether |
| CN114702407A (en) * | 2022-03-28 | 2022-07-05 | 浙江锦华新材料股份有限公司 | Method for synthesizing acetaldoxime by membrane reactor catalysis |
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| CN114702407A (en) * | 2022-03-28 | 2022-07-05 | 浙江锦华新材料股份有限公司 | Method for synthesizing acetaldoxime by membrane reactor catalysis |
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