CN105906487A - Refining method of polymethoxy dialkyl ether - Google Patents
Refining method of polymethoxy dialkyl ether Download PDFInfo
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- CN105906487A CN105906487A CN201610306274.2A CN201610306274A CN105906487A CN 105906487 A CN105906487 A CN 105906487A CN 201610306274 A CN201610306274 A CN 201610306274A CN 105906487 A CN105906487 A CN 105906487A
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- Prior art keywords
- formaldehyde
- dialkyl ether
- polymethoxy dialkyl
- synthetic product
- polymethoxy
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a refining method of polymethoxy dialkyl ether. By a chemical adsorption-desorption method, formaldehyde in a synthetic product is firstly adsorbed on an alkaline adsorption material; the effect of removing the formaldehyde in the synthetic product is achieved; after the adsorption saturation, the formaldehyde is desorbed by a temperature rise adsorption method; the adsorption material is regenerated; the operations are circulated in such a way. By adopting the method, the refining method has the advantages that the polymethoxy dialkyl ether synthetic product is refined; the subsequent product separation is favorably realized; meanwhile, a part of unreacted formaldehyde is recovered; the formaldehyde utilization rate is improved; the production cost is reduced, so that the industrial realization is facilitated.
Description
Technical field
The invention belongs to derived energy chemical technical field, be specifically related to the process for purification of a kind of polymethoxy dialkyl ether.
Background technology
The endowment of resources of China's " rich coal, gas oil-poor, few " relatively, makes economic society development lasting, very fast and oil supply
Contradiction.Since within 1993, becoming net import of oil state, import volume the most quickly increases, after 2009 externally
Interdependency alreadys more than 50%, imported crude oil 2.39 hundred million tons in 2010, within 2009, increases by 17.5% on year-on-year basis, has a strong impact on country
Energy strategy safety.Therefore, the reality constructs produced with primary energy from China's energy strategy safety, endowment of resources, send out
Exhibition non-petroleum base liquid fuel synthetic technology has strategic significance undoubtedly.
It addition, along with economic sustained and rapid development, China has become methanol production and has consumed fastest-rising country,
2000-2009 methanol output increases by 21.4% every year, does not obtain further development and utilization due to Downstream Products of Methanol,
The swift and violent methanol production capacity increased is considerably beyond the market demand.2013, the methanol device utilization of capacity was only 51.91%, and methanol produces
Can be serious superfluous, it is therefore desirable to extend Chemical Industry chain further.Methanol-based alternative fuel has caused extensively weight in China
Depending on.
Polyoxymethylene dialkyl ether (PODE) is with methylene epoxide as main chain, the low relative molecular mass contracting of low-carbon alkyl end-blocking
Aldehyde polymer, formula mostly is R1O(CH2O)n R2, wherein, R1And R2For CnH2n+1Or CnH2n, R1And R2Can be same base group, also
Can be different groups.Wherein, (polymethoxy methylal, english abbreviation are had another name called with the polymethoxy dimethyl ether of methyl blocking
DMMn, n=2～8), its formula is CH3(OCH2)nOCH3, for high boiling point yellow liquid, average Cetane number reaches more than 76,
Oxygen content is 47%～50%, and boiling point is about 160-280 DEG C, is a kind of cleaning, high cetane number diesel oil blending component, is also mesh
The environmental protection fuel oil component generally acknowledged on former world.Because polyoxymethylene dialkyl ether Cetane number is high, physical property is close with diesel oil, so
It is blended in diesel oil and is used without the engine fuel system of In-Use Motor Vehicles is made any change.
Polymethoxy dialkyl ether is with many with one or more in low-carbon alcohols (C1-C5) or low-carbon alkene or dimethoxym ethane
Polyformaldehyde/metaformaldehyde/formalin reacts under the catalyst action of acidic catalyst.This reaction is for reversible micro-
Exothermic reaction.Owing to reaction is affected by thermodynamical equilibrium, the conversion ratio of raw material paraformaldehyde/metaformaldehyde/formalin is only
50%-70% can be reached, have formaldehyde the most in the product.If the formaldehyde of remaining 30%-50% by alkali cleaning,
The method removings such as extraction, then can cause the waste wholly or in part of formaldehyde, thus cause increasing substantially of cost, can make simultaneously
Become substantial amounts of contaminated wastewater, be unfavorable for industrialized popularization.
Summary of the invention
In order to solve the drawbacks described above of prior art.The present invention provides techniques below scheme:
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether, its reaction expression is:
(2) polymethoxy dialkyl ether is refined: entered by pumping by the polymethoxy dialkyl ether synthetic product of preparation
In formaldehyde absorbing tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to
On absorption carrier, synthetic product air speed in adsorption tower is 0.5h-1—2.0h-1, adsorption temp is 10 DEG C-100 DEG C, absorption
The saturated rear PARA FORMALDEHYDE PRILLS(91,95) of tower carries out being desorbed in situ, uses the mode heated up to make adsorbing material release formaldehyde, and at 40 DEG C-150 DEG C
Carry out desorption and regeneration.
Described absorption carrier is one or more in silica gel, fiber, resin or activated carbon.
Modifying agent active group is amino, and modifying agent is MEA, dimethylamine, diethanolamine, N methyldiethanol amine,
2-amino 2-methyl isophthalic acid propanol or the Organic substance of other any band amino.
The Advantageous Effects of the present invention: the present invention method by chemisorbed-desorption, by the formaldehyde in synthetic product
First be adsorbed on alkaline adsorption material, play the effect of formaldehyde in removing synthetic product, adsorb saturated after, then pass through desorption by heating
Method make formaldehyde be desorbed, regenerative adsorption material, so circulate.In this way, not only polymethoxy dialkyl ether is closed
Product is become to be refined, the beneficially separation of subsequent product, reclaim a part of unreacted formaldehyde simultaneously, improve formaldehyde and utilize
Rate, reduction production cost, thus the most industrialized realization.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the preferred embodiments of the present invention.
Embodiment 1
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether.Its reaction expression is:
(2) polymethoxy dialkyl ether is refined: entered by pumping by the polymethoxy dialkyl ether synthetic product of preparation
In formaldehyde absorbing tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to
On absorption carrier, described adsorbing material is the silica gel through monoethanolamine modification, and synthetic product air speed in adsorption tower is 0.5h-1, adsorption temp is 10 DEG C, and the saturated rear PARA FORMALDEHYDE PRILLS(91,95) of adsorption tower carries out being desorbed in situ, uses the mode heated up to make adsorbing material discharge
Formaldehyde, and at 150 DEG C, carry out desorption and regeneration.Before and after absorption, in synthetic product, content of formaldehyde and formaldehyde utilization rate refer to table 1.
Embodiment 2
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether.Its reaction expression is:
(2) polymethoxy dialkyl ether is refined: will prepare polymethoxy dialkyl ether synthetic by pump inhaled formaldehyde
In adsorption tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to absorption
On carrier, described adsorbing material is the fiber through diethanolamine modification, and synthetic product air speed in adsorption tower is 2h-1, absorption
Temperature is 100 DEG C, and the saturated rear PARA FORMALDEHYDE PRILLS(91,95) of adsorption tower carries out being desorbed in situ, uses the mode heated up to make adsorbing material release formaldehyde,
And at 40 DEG C, carry out desorption and regeneration.Before and after absorption, in synthetic product, content of formaldehyde and formaldehyde utilization rate refer to table 1.
Embodiment 3
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether.Its reaction expression is:
(2) polymethoxy dialkyl ether is refined: enter first by preparing polymethoxy dialkyl ether synthetic product by pumping
In aldehyde adsorption tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to inhale
On appendix body, described adsorbing material is the resin through N methyldiethanol amine modification, and synthetic product air speed in adsorption tower is
1.5h-1, adsorption temp is 40 DEG C, and the saturated rear PARA FORMALDEHYDE PRILLS(91,95) of adsorption tower carries out being desorbed in situ, uses the mode heated up to make adsorbing material
Release formaldehyde, and at 100 DEG C, carry out desorption and regeneration.Before and after absorption, in synthetic product, content of formaldehyde and formaldehyde utilization rate refer to table
1。
Embodiment 4
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether.Its reaction expression is:
(2) polymethoxy dialkyl ether is refined: enter first by preparing polymethoxy dialkyl ether synthetic product by pumping
In aldehyde adsorption tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to inhale
On appendix body, described adsorbing material is the activated carbon through the modification of 2-amino 2-methyl isophthalic acid propanol, and synthetic product is in adsorption tower
Air speed is 1h-1, adsorption temp is 60 DEG C, and the saturated rear PARA FORMALDEHYDE PRILLS(91,95) of adsorption tower carries out being desorbed in situ, uses the mode heated up to make absorption
Material release formaldehyde, and at 80 DEG C, carry out desorption and regeneration.Before and after absorption, in synthetic product, content of formaldehyde and formaldehyde utilization rate are detailed
It is shown in Table 1.
Embodiment 5
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether.Its reaction expression is:
(2) polymethoxy dialkyl ether is refined: enter first by preparing polymethoxy dialkyl ether synthetic product by pumping
In aldehyde adsorption tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to inhale
On appendix body, described adsorbing material is the silica gel through N methyldiethanol amine modification, and synthetic product air speed in adsorption tower is
0.5h-1, adsorption temp is 80 DEG C, and the saturated rear PARA FORMALDEHYDE PRILLS(91,95) of adsorption tower carries out being desorbed in situ, uses the mode heated up to make adsorbing material
Release formaldehyde, and at 60 DEG C, carry out desorption and regeneration.Before and after absorption, in synthetic product, content of formaldehyde and formaldehyde utilization rate refer to table
1。
Embodiment 6
The process for purification of a kind of polymethoxy dialkyl ether, comprises the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: employing ethanol, propanol, butanol, amylalcohol and paraformaldehyde,
Metaformaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy two in tank reactor
Alkyl ether.Its reaction expression is:
(2) polymethoxy dialkyl ether is refined: will prepare polymethoxy dialkyl ether synthetic by pump inhaled formaldehyde
In adsorption tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to absorption
On carrier, described adsorbing material is the activated carbon through monoethanolamine modification, and synthetic product air speed in adsorption tower is 0.5h-1,
Adsorption temp is 90 DEG C, and the saturated rear PARA FORMALDEHYDE PRILLS(91,95) of adsorption tower carries out being desorbed in situ, uses the mode heated up to make adsorbing material discharge first
Aldehyde, and at 120 DEG C, carry out desorption and regeneration.Before and after absorption, in synthetic product, content of formaldehyde and formaldehyde utilization rate refer to table 1.
Content of formaldehyde and formaldehyde utilization rate in synthetic product before and after table 1 absorption
Formaldehyde in synthetic product can be greatly reduced after chemisorbed piptonychia aldehyde as can be seen from Table 1, play very
The effect of good purified product, improves the utilization rate of formaldehyde simultaneously, reduces production cost accordingly.
The present invention method by chemisorbed-desorption, is first adsorbed in alkaline adsorption material by the formaldehyde in synthetic product
On, play the effect of formaldehyde in removing synthetic product, adsorb saturated after, then make formaldehyde be desorbed by the method for desorption by heating, then
Raw adsorbing material, so circulates.In this way, not only polymethoxy dialkyl ether synthetic product is refined, profit
In the separation of subsequent product, reclaim a part of unreacted formaldehyde simultaneously, improve formaldehyde utilization rate, reduce production cost, thus
It is beneficial to industrialized realization.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (3)
1. the process for purification of a polymethoxy dialkyl ether, it is characterised in that: comprise the steps:
(1) preparation of polymethoxy dialkyl ether synthetic product: use ethanol, propanol, butanol, amylalcohol and paraformaldehyde, trimerization
Formaldehyde, formalin are raw material, under acidic catalyst effect, catalyze and synthesize polymethoxy dialkyl group in tank reactor
Ether, its reaction expression is:
(2) polymethoxy dialkyl ether is refined: by the polymethoxy dialkyl ether synthetic product of preparation by pump inhaled formaldehyde
In adsorption tower, having adsorbing material, described adsorbing material to include absorption carrier and modifying agent in adsorption tower, modifying agent is attached to absorption
On carrier, synthetic product air speed in adsorption tower is 0.5h-1—2.0h-1, adsorption temp is 10 DEG C-100 DEG C, and adsorption tower is satisfied
Carry out being desorbed in situ with rear PARA FORMALDEHYDE PRILLS(91,95), use the mode heated up to make adsorbing material release formaldehyde, and carry out at 40 DEG C-150 DEG C
Desorption and regeneration.
The process for purification of polymethoxy dialkyl ether the most according to claim 1, it is characterised in that: described absorption carrier is
Silica gel, fiber, resin or activated carbon in one or more.
The process for purification of polymethoxy dialkyl ether the most according to claim 1, it is characterised in that: modifying agent active group
For amino, modifying agent is MEA, dimethylamine, diethanolamine, N methyldiethanol amine, 2-amino 2-methyl isophthalic acid propanol or its
The Organic substance of its any band amino.
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| CN201610306274.2A CN105906487A (en) | 2016-05-10 | 2016-05-10 | Refining method of polymethoxy dialkyl ether |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096065A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The method of purification of polyoxymethylene dimethyl ethers |
| CN109096064A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The refining methd of polyoxymethylene dimethyl ethers |
| CN112374971A (en) * | 2020-11-12 | 2021-02-19 | 四川达兴能源有限责任公司 | Production method of polymethoxy dialkyl ether |
| CN112808237A (en) * | 2020-12-31 | 2021-05-18 | 桐乡市健民过滤材料有限公司 | Modified activated carbon fiber felt and filter screen for removing formaldehyde and preparation method thereof |
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| CN109096065A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The method of purification of polyoxymethylene dimethyl ethers |
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| CN112374971A (en) * | 2020-11-12 | 2021-02-19 | 四川达兴能源有限责任公司 | Production method of polymethoxy dialkyl ether |
| CN112808237A (en) * | 2020-12-31 | 2021-05-18 | 桐乡市健民过滤材料有限公司 | Modified activated carbon fiber felt and filter screen for removing formaldehyde and preparation method thereof |
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Inventor after: Xiong Chunhua Inventor after: Shang Hongyan Inventor after: An Gaojun Inventor after: Lu Changbo Inventor after: Xue Zhenzhen Inventor after: Wang Xudong Inventor after: Zhou Youjie Inventor before: An Gaojun Inventor before: Shang Hongyan Inventor before: Lu Changbo Inventor before: Xiong Chunhua Inventor before: Xue Zhenzhen Inventor before: Wang Xudong Inventor before: Zhou Youjie |
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Application publication date: 20160831 |