CN104725202A - Process device and method for production of poly methoxy dimethyl ether raw material - Google Patents
Process device and method for production of poly methoxy dimethyl ether raw material Download PDFInfo
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- CN104725202A CN104725202A CN201510128372.7A CN201510128372A CN104725202A CN 104725202 A CN104725202 A CN 104725202A CN 201510128372 A CN201510128372 A CN 201510128372A CN 104725202 A CN104725202 A CN 104725202A
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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
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/85—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process device and method for production of poly methoxy dimethyl ether raw material. The device comprises a deacidification device, a reaction layering device, a dehydrating tower and a raw material tower which are connected in sequence, wherein a preheater is arranged between the deacidification device and the reaction layering device, vacuum extraction equipment is arranged at the top of the dehydrating tower, a stripping reaction decomposition section is arranged at the lower part of the raw material tower, the upper part of the raw material tower is a returned material mixing section and is provided with poly methoxy dimethyl ether reaction raw material return inlet, and the bottom of the raw material tower is connected with the reaction layering device through a pipeline. According to the method, formaldehyde solution which is low in cost is used as a basic raw material to prepare poly methoxy dimethyl ether production raw material; moreover, after the raw material prepared according to the process method is mixed with methylal and then is processed through a fixed bed reactor, the conversion rate is high and the selectivity for DMM3-8 products is high.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to producing and manufacturing technique and the device of polymethoxy dimethyl ether.
Background technology
(Chinese also can be polyoxymethylene dimethyl ether to polymethoxy dimethyl ether, polyoxymethylene dimethyl ethers, polymethoxy methylal, polyoxymethylene dimethyl ethers etc.), i.e. polyoxymethylene dimethyl ethers (PODE), it is the common name of a class material, and its molecular structural formula is CH
3o (CH
2o) nCH
3, there is higher cetane value (cetane number, CN.When n=3 ~ 8, CN>76) and oxygen level (42 ~ 49%).When the value of n is 3 ~ 8, its physical and chemical performance, combustionproperty and diesel oil closely, can be used as diesel-dope, and the addition in diesel oil can reach 30% (v/v), keeps higher cetane value and combustionproperty simultaneously.The oilness of diesel oil can be improved, reduce combustion fumes and generate, diesel oil combustion position within the engine can be improved, improve thermo-efficiency, the particulate matter in reduction combustion tail gas and the discharge of NOx.Also possibility diesel oil substitute, directly as diesel-fuel.
The raw material that current polymethoxy dimethyl ether mainly adopts is paraformaldehyde, concentrated formaldehyde solution or trioxymethylene and methylal.Because paraformaldehyde and trioxymethylene are solid formaldehyde, reaction conditions is harsher, the relatively high general control of reaction pressure is at 1 ~ 2.5MPa, thus cause equipment cost high, and the reaction of solid formaldehyde and methylal generally adopts suspension bed and fluidized-bed reactor, catalyzer life cycle is short, the large and trioxymethylene of loss and paraformaldehyde raw materials cost high; Concentrated formaldehyde solution is raw material, cause being that the transformation efficiency of raw material reaction polymethoxy dimethyl ether is relatively low with concentrated formaldehyde due to the existence of water in reaction process, more difficult and product separation energy consumption is also higher to product separation, and above-mentioned reaction is not high for the selectivity of DMM3 ~ 8 product.
Summary of the invention
Goal of the invention: for above-mentioned Problems existing and defect, the invention provides a kind of process unit for polymethoxy dimethyl ether raw material production and processing method, with 37 ~ 50% more cheap formaldehyde solutions for basic raw material, prepare the raw material that polymethoxy dimethyl ether is produced.And by fixed-bed reactor after mixing with methylal according to the raw material that this technique obtains, transformation efficiency is high, and high for the selectivity of DMM3 ~ 8 product.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of process unit for polymethoxy dimethyl ether raw material production, comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, wherein: be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, described in carry the bottom of heating up in a steamer reaction decomposes section and be connected with reaction decker by pipeline.
As preferably, described deacidifying device is ion exchange tower.
As preferably, the exchang medium of filling in described deacidifying device is silica gel or weak base anion-exchange resin.
Present invention also offers a kind of polymethoxy dimethyl ether technique for producing raw material method based on above-mentioned process unit, comprise the following steps:
(1) using formaldehyde solution as raw material, and through depickling process, in control solution, acid content is lower than 10ppm;
(2) send into after the formaldehyde solution after depickling being preheated to 60 ~ 100 DEG C in reaction decker, add auxiliary and mix, the raw material midbody making formaldehyde and auxiliary be obtained by reacting water insoluble and density to be less than water, and stratification;
(3) extract the supernatant liquid leaving standstill liquid out and send into dehydration tower, and through vacuum hydro-extraction process, remove the moisture in supernatant liquid;
(4) liquid after dehydration sends into raw material tower centre entrance again, and flowing through in the process carried and heat up in a steamer reaction decomposes section, at 160 ~ 220 DEG C, raw material midbody decomposition-reduction becomes formaldehyde gas and auxiliary liquid, formaldehyde gas upwards flows and contacts with the backflow material that polymethoxy dimethyl ether raw material reflux inlet enters and mass-and heat-transfer effect occurs, thus carry the reaction raw materials that backflow material obtains polymethoxy dimethyl ether, depart from from reaction system.
Further, described in step (2), auxiliary is monohydroxy-alcohol, dibasic alcohol or aldehydes matter.
Further, described auxiliary is unitary saturated alcohol or binary saturated alcohol.
Further, described auxiliary is one or more mixture in isopropylcarbinol, 4-methyl-2-amylalcohol or hexalin.
As preferably, the temperature of reaction in described reaction decker is 80 ~ 100 DEG C, and reaction time is 1 ~ 5h.
As preferably, in described dehydration tower, pressure is 20 ~ 100KPa, and service temperature is 60 ~ 100 DEG C.
As preferably, described raw material tower is distillation tower, and the temperature of tower bottom is 160 ~ 220 DEG C, and adopts backflow material dilution formaldehyde.
Beneficial effect: compared with prior art, the present invention directly uses the formaldehyde of 37 ~ 50% common concentration to be preparation of raw material, utilizes the feature of auxiliary and formaldehyde reaction, the raw material of configuration polymethoxy dimethyl ether.Because raw material is the most general formaldehyde solution in market, simple and easy to get, with low cost.The program carried out depickling process before reacting, and reduced acidity to auxiliary consumption in the reaction.And the program strictly controls the temperature in raw material tower, and adopt the raw material tower of this invention, considerably increase the reversed reaction time of subsystem and formaldehyde solution, thus again reduce the consumption of auxiliary.This raw material device not adopts the mode of conventional liquid of top of the tower backflow, but adopts the DMM2 in a large amount of DMM or polymethoxy dimethyl ether reaction product or reaction solution to reflux, and greatly increases the processing safety of this device.And the water of batching of the present invention directly only containing formaldehyde and DMM or DMM2, PPM level content, this raw material prepare polymethoxy dimethyl ether reaction conversion ratio and selectivity high.
Accompanying drawing explanation
Fig. 1 is the schema of polymethoxy dimethyl ether technique for producing raw material method of the present invention.
Wherein, deacidifying device 1, preheater 2, reaction decker 3, dehydration tower 4, vacuum extractor 5, raw material tower 6, liquid pump 7.
Embodiment
Below in conjunction with the drawings and specific embodiments, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
As shown in Figure 1, process unit for polymethoxy dimethyl ether raw material production of the present invention, comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, wherein: be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, described in carry the bottom of heating up in a steamer reaction decomposes section and be connected with reaction decker by pipeline.Major processes is as follows:
37 ~ 50% formaldehyde solutions market bought or produces, carry out depickling process through silica gel or macropore weak basic anion exchange resin, after depickling process, solution acid content is (1 ~ 10ppm).Formaldehyde solution after depickling process is by after being preheating to 60 ~ 100 DEG C, abundant hybrid reaction is carried out with auxiliary in reaction decker (adopting in tower or basin), reacted component due to density ratio water little, through leave standstill after, supernatant liquid through pump delivery to dehydration tower.Wherein said auxiliary is unitary saturated alcohol or binary saturated alcohol and ether material, one in preferred isopropylcarbinol, 4-methyl-2-amylalcohol or hexalin, in fact the unitary saturated alcohol equal prodigiosin of carbonatoms between 3 ~ 9 and formaldehyde form reaction product that is water-fast but easily thermolysis, but there are differences in concrete heat decomposition temperature and transformation efficiency.
The reaction product obtained in reaction decker has thermolysis effect, and dehydration tower controls at vacuum operating, and moisture is deviate from by the tower top that dewaters, and by being pumped into raw material tower bottom dehydration tower, the working pressure in dehydration tower is 20 ~ 100KPa.In raw material tower, lower end is mainly stripping section and reactant decomposition section, control this section of temperature 120 ~ 160 DEG C, upper end is by supplementing the DMM2 component backflow in methylal or polymethoxy dimethyl ether product, obtain methylal and formaldehyde (or mix products of DMM2 and formaldehyde) at raw material tower top, direct gas phase is as the reaction raw materials of polymethoxy dimethyl ether.Be auxiliary bottom raw material tower, by being pumped into reaction unit recycle.
Above production method mainly includes deacidifying device, mixed reactor, dewatering unit, raw material preparation facilities.Major control index, in charging formaldehyde, acid content can not more than 1000ppm; Hybrid reaction controls temperature of reaction 80 ~ 100 DEG C, reaction time 1 ~ 5h; Dehydration tower red-tape operati pressure 20 ~ 100KPa (A), service temperature controls 60 ~ 100 DEG C; Raw material tower controls pressure-fired, and tower top service temperature controls 90 ~ 120 DEG C, and tower reactor section temperature is 160 ~ 220 DEG C.Wherein raw material tower is rectifying tower, the region residence time long Reaction Separation being beneficial to formaldehyde and auxiliary system of major control tower reactor section 140 ~ 200 DEG C, thus formaldehyde can depart from by reaction system, and the transformation efficiency that formaldehyde departs from is high, because the formaldehyde gas detached 100 ~ 120 DEG C time is easily polymerized in tower, therefore adopt the material of boiling point in this region to carry out the concentration refluxing to dilute formaldehyde, prevent polymerization.This backflow adopts the DMM2 in a large amount of DMM or polymethoxy dimethyl ether reaction product or reaction solution to reflux, and adopts this system to reflux the DMM2 selectivity that can also effectively improve in reaction system.
Claims (10)
1. the process unit for polymethoxy dimethyl ether raw material production, it is characterized in that: comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, wherein: be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, described in carry the bottom of heating up in a steamer reaction decomposes section and be connected with reaction decker by pipeline.
2. process unit according to claim 1, is characterized in that: described deacidifying device is ion exchange tower.
3. process unit according to claim 2, is characterized in that: the exchang medium of filling in described deacidifying device is silica gel or weak base anion-exchange resin.
4., based on a polymethoxy dimethyl ether technique for producing raw material method for the arbitrary described process unit of claims 1 to 3, it is characterized in that comprising the following steps:
(1) using formaldehyde solution as raw material, and through depickling process, in control solution, acid content is lower than 10ppm;
(2) send into after the formaldehyde solution after depickling being preheated to 60 ~ 100 DEG C in reaction decker, add auxiliary and mix, the raw material midbody making formaldehyde and auxiliary be obtained by reacting water insoluble and density to be less than water, and stratification;
(3) extract the supernatant liquid leaving standstill liquid out and send into dehydration tower, and through vacuum hydro-extraction process, remove the moisture in supernatant liquid;
(4) liquid after dehydration sends into raw material tower centre entrance again, and flowing through in the process carried and heat up in a steamer reaction decomposes section, at 160 ~ 220 DEG C, raw material midbody decomposition-reduction becomes formaldehyde gas and auxiliary liquid, formaldehyde gas upwards flows and contacts with the backflow material that polymethoxy dimethyl ether raw material reflux inlet enters and mass-and heat-transfer effect occurs, thus carry the reaction raw materials that backflow material obtains polymethoxy dimethyl ether, depart from from reaction system.
5. processing method according to claim 4, is characterized in that: described in step (2), auxiliary is monohydroxy-alcohol, dibasic alcohol or aldehydes matter.
6. processing method according to claim 5, is characterized in that: described auxiliary is unitary saturated alcohol or binary saturated alcohol.
7. processing method according to claim 6, is characterized in that: described auxiliary is one or more mixture in isopropylcarbinol, 4-methyl-2-amylalcohol or hexalin.
8. processing method according to claim 4, it is characterized in that: the temperature of reaction in described reaction decker is 80 ~ 100 DEG C, reaction time is 1 ~ 5h.
9. processing method according to claim 4, it is characterized in that: in described dehydration tower, pressure is 20 ~ 100KPa, service temperature is 60 ~ 100 DEG C.
10. processing method according to claim 4, it is characterized in that: described raw material tower is distillation tower, the temperature of tower bottom is 160 ~ 220 DEG C, and adopts backflow material dilution formaldehyde.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510128372.7A CN104725202A (en) | 2015-03-24 | 2015-03-24 | Process device and method for production of poly methoxy dimethyl ether raw material |
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| CN201510128372.7A CN104725202A (en) | 2015-03-24 | 2015-03-24 | Process device and method for production of poly methoxy dimethyl ether raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278836A (en) * | 2016-08-16 | 2017-01-04 | 鄂尔多斯市易臻石化科技有限公司 | Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether |
| CN113087603A (en) * | 2020-01-09 | 2021-07-09 | 中国石油化工股份有限公司 | Production system and production method of polymethoxy dimethyl ether |
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| US2848500A (en) * | 1957-01-28 | 1958-08-19 | Du Pont | Preparation of purified formaldehyde |
| US3423368A (en) * | 1965-10-14 | 1969-01-21 | Hary E Cier | Extractive recovery of formaldehyde |
| EP0543226A2 (en) * | 1991-11-16 | 1993-05-26 | BASF Aktiengesellschaft | Process for the preparation of anhydrous and from impurities depleted formaldehyde |
| US6229053B1 (en) * | 1997-10-31 | 2001-05-08 | Ticona Gmbh | Method for purification of formaldehyde, use thereof and plastics produced therewith |
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| CN103848730A (en) * | 2014-01-09 | 2014-06-11 | 东营市润成碳材料科技有限公司 | Production device system and production process for polymethoxy dimethyl ether (PODE) |
| CN204079853U (en) * | 2014-09-04 | 2015-01-07 | 北京旭阳化工技术研究院有限公司 | For the production of the reaction unit of polymethoxy dimethyl ether |
| CN204569779U (en) * | 2015-03-24 | 2015-08-19 | 江苏凯茂石化科技有限公司 | A kind of process unit for polymethoxy dimethyl ether raw material production |
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2015
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Patent Citations (9)
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| GB752163A (en) * | 1953-07-16 | 1956-07-04 | Du Pont | Preparation of purified formaldehyde |
| US2848500A (en) * | 1957-01-28 | 1958-08-19 | Du Pont | Preparation of purified formaldehyde |
| US3423368A (en) * | 1965-10-14 | 1969-01-21 | Hary E Cier | Extractive recovery of formaldehyde |
| EP0543226A2 (en) * | 1991-11-16 | 1993-05-26 | BASF Aktiengesellschaft | Process for the preparation of anhydrous and from impurities depleted formaldehyde |
| US6229053B1 (en) * | 1997-10-31 | 2001-05-08 | Ticona Gmbh | Method for purification of formaldehyde, use thereof and plastics produced therewith |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278836A (en) * | 2016-08-16 | 2017-01-04 | 鄂尔多斯市易臻石化科技有限公司 | Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether |
| CN113087603A (en) * | 2020-01-09 | 2021-07-09 | 中国石油化工股份有限公司 | Production system and production method of polymethoxy dimethyl ether |
| CN113087603B (en) * | 2020-01-09 | 2022-12-09 | 中国石油化工股份有限公司 | Production system and production method of polymethoxy dimethyl ether |
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Effective date of registration: 20170428 Address after: Jinxi road Binhu District 214000 Jiangsu city of Wuxi province No. 100 Applicant after: WUXI ZHIGUI TECHNOLOGY CO., LTD. Address before: No. 58 Henghua Technology Park 214000 Jiangsu province Binhu District of Wuxi City Xiu Xi Lu (big river No. 50 South Gate) Applicant before: Jiangsu Kaimao Chemical Technology Co., Ltd. |
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