CN105541570A - Process for preparing Polyoxymethylene dimethyl ether through acetalization reaction - Google Patents
Process for preparing Polyoxymethylene dimethyl ether through acetalization reaction Download PDFInfo
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- CN105541570A CN105541570A CN201410592995.5A CN201410592995A CN105541570A CN 105541570 A CN105541570 A CN 105541570A CN 201410592995 A CN201410592995 A CN 201410592995A CN 105541570 A CN105541570 A CN 105541570A
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- formaldehyde
- trioxymethylene
- acid root
- acetalation
- dimethyl ether
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a process for preparing polyoxymethylene dimethyl ether through an acetalization reaction. According to the present invention, the process comprises the following two steps that under the catalysis effect of an ionic liquid ILI, a formaldehyde aqueous solution is subjected to a polymerization reaction to obtain a mixed aqueous solution of trioxymethylene and formaldehyde, and under the catalysis effect of an ionic liquid ILII, the mixed aqueous solution of trioxymethylene and formaldehyde and methanol are subjected to an acetalization reaction to prepare the polyoxymethylene dimethyl ether. According to the present invention, the formaldehyde aqueous solution is adopted as the initial reaction raw material, the continuous polymerization and the acetalization reaction are used to prepare the polyoxymethylene dimethyl ether, and the formaldehyde utilization rate is high; the film type evaporator is used, such that the rapid separation and the recycling of the light components are achieved, and the separation efficiency is high; and the catalyst separation is simple, and the catalyst recycling is achieved.
Description
Technical field
The invention belongs to chemical technique field, be specifically related to the technological process that a kind of acetalation prepares polymethoxy dimethyl ether.
Background technology
The technological process that acetalation prepares polymethoxy dimethyl ether at least comprises the primary processes such as catalyst preparing, rectifying, separation.Prepare in the technological process method of polymethoxy dimethyl ether in current preparation acetalation, technical process is not easy to implement, and separation efficiency is low, can not achieve recycling of catalyzer, and production process is complicated, and production efficiency is low.
Summary of the invention
In order to overcome the above-mentioned technical problem that prior art field exists, the object of the invention is to, there is provided a kind of acetalation to prepare the technological process of polymethoxy dimethyl ether, the present invention not only production process simple, increase work efficiency, and achieve recycling of catalyzer.
Acetalation provided by the invention prepares the technological process of polymethoxy dimethyl ether, comprises the following steps:
(1) oxymethylene polymerization reactive distillation district, comprises a reaction and rectification device, gas phase condenser; With acidic ion liquid ILI for catalyzer, adopt 40-60wt% formalin, 80-110 DEG C, there is successive polymerization reaction under 1.0-0.1Mpa and generate trioxymethylene, from the azeotrope that reaction and rectification device expellant gas is trioxymethylene, formaldehyde and water, the trioxymethylene containing 30-50wt%, the formaldehyde containing 20-30wt%; Enter gas phase condenser V6 after gas collection, after condensation, enter acetalation device R2; The cationic moiety of acidic ion liquid ILI be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one in pyridylium or heterocyclic onium cations, anionicsite is selected from the one in p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid root, bisulfate ion, trifluoroacetic acid root;
(2) acetalation districts, in a single-stage or Multi-stage stirring reactor; With acidic ion liquid ILII for catalyzer, trioxymethylene, formaldehyde mixture and methyl alcohol 100-140 DEG C, carry out continuous acetalation under 0.5-4.0Mpa; The reactor stream fluid flowed out continuously in reaction zone, except containing except the DMM16 generated, water, also containing above-mentioned unreacting material and catalyzer; The cationic moiety of acidic ion liquid ILII be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one in pyridylium and heterocyclic onium cations, anionicsite is selected from the one in p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid root, bisulfate ion and trifluoroacetic acid root;
(3) disengaging zone, comprise single-stage or Multistage rectifying tower, film-type evaporator and phase separator, are composed in series; From the reactor stream fluid that above-mentioned acetalation district flows out, step-down, continuously flow into rectifying tower, evaporation, condensation under nitrogen protection, be separated into light constituent a1, a1 represents formaldehyde, methyl alcohol, trioxymethylene, DMM16 and water, and recycling catalyst two bursts of logistics, and recycling catalyst returns to acetalation device; Light constituent a1 continuously flows into film-type evaporator, evaporation, condensation under nitrogen protection, isolate light constituent b1, b1 represents DMM12, formaldehyde, methyl alcohol, trioxymethylene and part water, the mixed solution of DMM36 and water continuously flows into phase separator again, is separated into product phase and aqueous phase two stream stock; Product is mainly containing DMM36.
Acetalation provided by the invention prepares the technological process of polymethoxy dimethyl ether, and its beneficial effect is, overcoming prior art, to prepare operation in the technological process of polymethoxy dimethyl ether more, and the problem that workload is large, improves working efficiency; Improve the utilization ratio of catalyzer.
Embodiment
Below in conjunction with an embodiment, the technological process being prepared by acetalation provided by the invention to polymethoxy dimethyl ether is described in detail.
Embodiment
The acetalation of the present embodiment prepares the technological process of polymethoxy dimethyl ether, comprises the following steps:
(1) oxymethylene polymerization reactive distillation district, comprises a reaction and rectification device, gas phase condenser; With acidic ion liquid ILI for catalyzer, adopt 50wt% formalin, 90 DEG C, there is successive polymerization reaction under 0.1Mpa and generate trioxymethylene, from the azeotrope that reaction and rectification device expellant gas is trioxymethylene, formaldehyde and water, the trioxymethylene containing 50wt%, the formaldehyde containing 20wt%; Enter gas phase condenser V6 after gas collection, after condensation, enter acetalation device R2; The cationic moiety of acidic ion liquid ILI be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one in pyridylium or heterocyclic onium cations, anionicsite is selected from the one in p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid root, bisulfate ion, trifluoroacetic acid root;
(2) acetalation districts, in a single-stage or Multi-stage stirring reactor; With acidic ion liquid ILII for catalyzer, trioxymethylene, formaldehyde mixture and methyl alcohol 100 DEG C, carry out continuous acetalation under 4.0Mpa; The reactor stream fluid flowed out continuously in reaction zone, except containing except the DMM16 generated, water, also containing above-mentioned unreacting material and catalyzer; The cationic moiety of acidic ion liquid ILII be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one in pyridylium and heterocyclic onium cations, anionicsite is selected from the one in p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid root, bisulfate ion and trifluoroacetic acid root;
(3) disengaging zone, comprise single-stage or Multistage rectifying tower, film-type evaporator and phase separator, are composed in series; From the reactor stream fluid that above-mentioned acetalation district flows out, step-down, continuously flow into rectifying tower, evaporation, condensation under nitrogen protection, be separated into light constituent a1, a1 represents formaldehyde, methyl alcohol, trioxymethylene, DMM16 and water, and recycling catalyst two bursts of logistics, and recycling catalyst returns to acetalation device; Light constituent a1 continuously flows into film-type evaporator, evaporation, condensation under nitrogen protection, isolate light constituent b1, b1 represents DMM12, formaldehyde, methyl alcohol, trioxymethylene and part water, the mixed solution of DMM36 and water continuously flows into phase separator again, is separated into product phase and aqueous phase two stream stock; Product is mainly containing DMM36.
Acetalation prepares the technological process of polymethoxy dimethyl ether, directly acetalation can prepare polymethoxy dimethyl ether, and without the need to further processing, operation is simple, and take off data is accurate, easy to implement.
Claims (1)
1. acetalation prepares a technological process for polymethoxy dimethyl ether, it is characterized in that: said method comprising the steps of:
(1) oxymethylene polymerization reactive distillation district, comprises a reaction and rectification device, gas phase condenser; With acidic ion liquid ILI for catalyzer, adopt 40-60wt% formalin, 80-110 DEG C, there is successive polymerization reaction under 1.0-0.1Mpa and generate trioxymethylene, from the azeotrope that reaction and rectification device expellant gas is trioxymethylene, formaldehyde and water, the trioxymethylene containing 30-50wt%, the formaldehyde containing 20-30wt%; Enter gas phase condenser V6 after gas collection, after condensation, enter acetalation device R2; The cationic moiety of acidic ion liquid ILI be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one in pyridylium or heterocyclic onium cations, anionicsite is selected from the one in p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid root, bisulfate ion, trifluoroacetic acid root;
(2) acetalation districts, in a single-stage or Multi-stage stirring reactor; With acidic ion liquid ILII for catalyzer, trioxymethylene, formaldehyde mixture and methyl alcohol 100-140 DEG C, carry out continuous acetalation under 0.5-4.0Mpa; The reactor stream fluid flowed out continuously in reaction zone, except containing except the DMM16 generated, water, also containing above-mentioned unreacting material and catalyzer; The cationic moiety of acidic ion liquid ILII be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one in pyridylium and heterocyclic onium cations, anionicsite is selected from the one in p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid root, bisulfate ion and trifluoroacetic acid root;
(3) disengaging zone, comprise single-stage or Multistage rectifying tower, film-type evaporator and phase separator, are composed in series; From the reactor stream fluid that above-mentioned acetalation district flows out, step-down, continuously flow into rectifying tower, evaporation, condensation under nitrogen protection, be separated into light constituent a1, a1 represents formaldehyde, methyl alcohol, trioxymethylene, DMM16 and water, and recycling catalyst two bursts of logistics, and recycling catalyst returns to acetalation device; Light constituent a1 continuously flows into film-type evaporator, evaporation, condensation under nitrogen protection, isolate light constituent b1, b1 represents DMM12, formaldehyde, methyl alcohol, trioxymethylene and part water, the mixed solution of DMM36 and water continuously flows into phase separator again, is separated into product phase and aqueous phase two stream stock; Product is mainly containing DMM36.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753666A (en) * | 2016-05-10 | 2016-07-13 | 中国人民解放军总后勤部油料研究所 | Method for preparing polyoxymethylene dimethyl ether |
| CN108329294A (en) * | 2018-04-10 | 2018-07-27 | 中国科学院成都有机化学有限公司 | Formaldehyde prepares the coupling process of metaformaldehyde |
| CN108383696A (en) * | 2018-04-24 | 2018-08-10 | 中国科学院成都有机化学有限公司 | The method for preparing polymethoxy dimethyl ether |
| CN110156575A (en) * | 2019-04-17 | 2019-08-23 | 天津大学 | Reactive distillation-Steam soak coupling technique for polymethoxy dimethyl ether synthesis |
-
2014
- 2014-10-30 CN CN201410592995.5A patent/CN105541570A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753666A (en) * | 2016-05-10 | 2016-07-13 | 中国人民解放军总后勤部油料研究所 | Method for preparing polyoxymethylene dimethyl ether |
| CN108329294A (en) * | 2018-04-10 | 2018-07-27 | 中国科学院成都有机化学有限公司 | Formaldehyde prepares the coupling process of metaformaldehyde |
| CN108383696A (en) * | 2018-04-24 | 2018-08-10 | 中国科学院成都有机化学有限公司 | The method for preparing polymethoxy dimethyl ether |
| CN108383696B (en) * | 2018-04-24 | 2021-01-12 | 中国科学院成都有机化学有限公司 | Method for preparing polymethoxy dimethyl ether |
| CN110156575A (en) * | 2019-04-17 | 2019-08-23 | 天津大学 | Reactive distillation-Steam soak coupling technique for polymethoxy dimethyl ether synthesis |
| CN110156575B (en) * | 2019-04-17 | 2023-06-06 | 天津大学 | Reactive distillation-vapor permeation coupling process for polymethoxy dimethyl ether synthesis |
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