CN104722249A - Multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and polyoxymethylene dimethyl ether synthesis process unit - Google Patents
Multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and polyoxymethylene dimethyl ether synthesis process unit Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 110
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 title claims abstract description 10
- -1 polyoxymethylene dimethyl ether Polymers 0.000 title abstract 6
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 95
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 40
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 24
- 239000000945 filler Substances 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 21
- 238000010521 absorption reaction Methods 0.000 claims description 15
- 238000012856 packing Methods 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 239000007792 gaseous phase Substances 0.000 claims description 11
- 238000007670 refining Methods 0.000 claims description 10
- 239000012295 chemical reaction liquid Substances 0.000 claims description 9
- 230000008676 import Effects 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 32
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 12
- 235000019253 formic acid Nutrition 0.000 description 12
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229930040373 Paraformaldehyde Natural products 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 229920002866 paraformaldehyde Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000006280 diesel fuel additive Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005829 trimerization reaction Methods 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- 239000002283 diesel fuel Substances 0.000 description 1
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- 230000032050 esterification Effects 0.000 description 1
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
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Abstract
The invention discloses a multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and a polyoxymethylene dimethyl ether synthesis process unit. A tower body of the multi-section reaction tower comprises at least two layers of reaction sections from top to bottom; each layer of reaction section is provided with a tower plate and forms a bent passageway; catalysts are arranged between the tower plates in a filling manner; gas ascension pipes are arranged between the adjacent layers of reaction sections; a gas phase outlet is formed in the tower top of the reaction tower; and each layer of reaction section is provided with an inlet with a valve and an outlet with a valve. According to the multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and the polyoxymethylene dimethyl ether synthesis process unit, the conversion equilibrium point of the reaction is effectively controlled, the advancement of the reaction equilibrium toward bigger polymers is effectively deferred, the conversion rate and the selectivity are improved, the reaction is carried out under the conditions that the catalyst activity is relatively high and the temperature does not excessively influence the reaction equilibrium, and good conversion rate and selectivity are obtained.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to manufacturing technique method and the device of polymethoxy dimethyl ether.
Background technology
The feature of China's energy resource structure is: rich coal, oil-poor, weak breath, and economic maintaining sustained and rapid growth is increasing to energy demand, the contradiction of society, expanding economy and oil supply.Since 2009, crude oil in China external dependence degree exceedes warning line (50%) in continuous 6 years, has a strong impact on the energy strategy safety of China.From China's energy strategy safety, in conjunction with China's primary energy structure feature, Development of Coal base liquid fuel synthetic technology has strategic significance undoubtedly.In addition, China's methyl alcohol production capacity is seriously superfluous, exploitation Downstream Products of Methanol, extends Chemical Industry chain, all has realistic meaning.
Polymethoxy dimethyl ether is a kind of universally acknowledged clean diesel component, its Cetane number >=70, not sulfur-bearing, aromatic-free.Add in diesel oil in 5%-20% ratio, can diesel cetane-number be improved, promote burning, reduce the discharge of the pernicious gases such as PM2.5, PM10, NOx, CO in vehicle exhaust significantly.Due to the excellent properties of polymethoxy dimethyl ether, its synthesis technique has become the heat subject of research both at home and abroad.At present, polymethoxy dimethyl ether is react under the catalytic action of acidic catalyst with one or more in methyl alcohol or dimethoxym ethane and formalin/metaformaldehyde/paraformaldehyde to generate mostly.And this reaction is exothermic reaction, the high reaction counter movement that causes of temperature, therefore needs to withdraw heat.No matter and be paraformaldehyde or metaformaldehyde all first need heating parse monomer formaldehyde could participate in reaction, therefore system reaction temperature is very high, general more than 110 DEG C, and the mode of pressurization must be adopted to prevent the lower dimethoxym ethane of boiling point and methanol gasifying, therefore cause that energy consumption is high, equipment requirement is high.In addition, under hot environment so, monomer formaldehyde has very high activity, disproportionated reaction easily occurs and produces a large amount of formic acid, if do not separated by formic acid in system, formic acid can be cumulative and bring significant negative impact to the molecular balance of polymethoxy dimethyl ether, cause the yield of reaction to reduce, therefore can only adopt in absorption or alkali and acid stripping method separating formic, cause complex process, and target product yield is low, synthesis cost is high.The amount of the selective and catalyst of product DMMn3-8 has close relationship, and common fixed bed cannot realize the adjustment product degree of polymerization, therefore causes n value too small or excessive, affects product quality.Test proves that the most applicable degree of polymerization making diesel fuel additives is the product of DMMn3-5.
Summary of the invention
Goal of the invention: for above-mentioned Problems existing and defect, the invention provides a kind of multisection type reaction tower for polymethoxy dimethyl ether and polymethoxy dimethyl ether synthesis technique device, solve the problem that at present, Synthesis conversion high with the cost brought in paraformaldehyde/trimerization production process and yield are low, and the present invention has the fixed bed reactors well removing thermal effect and adjustable product conversion degree, can promote that reaction is carried out efficiently, transforming degree achieves controllability.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of multisection type reaction tower for polymethoxy dimethyl ether synthesis, described reaction tower tower body comprises at least two-layer conversion zone from top to bottom, and every layer of conversion zone is provided with column plate and forms bending runner, catalyst is filled with between column plate, also be provided with vapor riser between the conversion zone of adjacent two layers, reaction tower tower top is also provided with gaseous phase outlet; Every layer of conversion zone is equipped with import and the outlet of band valve.
As preferably, described conversion zone has four layers.
Present invention also offers the process unit of a kind of gas formaldehyde synthesis polymethoxy dimethyl ether, comprise filler reaction tower, separation of products tower and multisection type reaction tower, wherein:
Described filler reaction tower is provided with the packing section being filled with catalyst, spray system and bubble absorption section respectively above and below packing section, described filler reaction tower be also provided with the dimethoxym ethane entrance be connected with spray system, the formaldehyde gas entrance be connected with bubble absorption section, bottom first order reaction liquid export and the gaseous phase outlet at top; Described bubble absorption section is also communicated with dimethoxym ethane entrance by tubing pump;
The bottom first order reaction liquid outlet of described filler reaction tower is connected with the entrance of separation of products tower (vacuum rectification tower), described separation of products tower also comprises the products export, the gaseous phase outlet of tower top and the light fraction outlet on tower top that are located at the bottom of tower, the light fraction outlet on described tower top is connected by the import of pipeline with multisection type reaction tower, and this passage is also provided with dimethoxym ethane supply pipe; And the outlet of multisection type reaction tower is communicated with by the entrance of pipeline with separation of products tower.
As preferably, the products export of described separation of products tower is also connected with refining rectifying column (vacuum rectification tower), this refining rectifying column also comprises the target product outlet that the heavy constituent be located at the bottom of tower exported, was located at tower top, and the pipeline of this target product outlet is provided with condenser.
As preferably, the gaseous phase outlet of described separation of products top of tower is communicated with the formaldehyde gas entrance of filler reaction tower by pipeline.
Beneficial effect: compared with prior art, the present invention has the following advantages: the abundant absorption effectively making formaldehyde gas and dimethoxym ethane, realizes bubble absorption integrated with catalytic reaction, improves the conversion ratio of formaldehyde; And utilize multisection type reactor, effectively control the inversion equilibrium point of reaction, effective prevention molecular balance is to the carrying out in larger polymer direction, improve conversion ratio and selective, make reaction higher and carry out under unduly affecting the temperature of molecular balance at catalyst activity, achieve good conversion ratio and selective.
Accompanying drawing explanation
Fig. 1 is the structural representation of the synthesis technique device of polymethoxy dimethyl ether of the present invention;
Fig. 2 is the structural representation of refining rectifying column process unit of the present invention.
Wherein, filler reaction tower 1, separation of products tower 2, multisection type reaction tower 3, refining rectifying column 4.
Detailed description of the invention
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, the process unit of gas formaldehyde synthesis polymethoxy dimethyl ether of the present invention, comprises filler reaction tower, separation of products tower and multisection type reaction tower, wherein:
Described filler reaction tower is provided with the packing section being filled with catalyst, spray system and bubble absorption section respectively above and below packing section, described filler reaction tower be also provided with the dimethoxym ethane entrance be connected with spray system, the formaldehyde gas entrance be connected with bubble absorption section, bottom first order reaction liquid export and the gaseous phase outlet at top; Described bubble absorption section is also communicated with dimethoxym ethane entrance by tubing pump;
The bottom first order reaction liquid outlet of described filler reaction tower is connected with the entrance of separation of products tower (vacuum rectification tower), described separation of products tower also comprises the products export, the gaseous phase outlet of tower top and the light fraction outlet on tower top that are located at the bottom of tower, the light fraction outlet on described tower top is connected by the import of pipeline with multisection type reaction tower, and this passage is also provided with dimethoxym ethane supply pipe; And the outlet of multisection type reaction tower is communicated with by the entrance of pipeline with separation of products tower.
Described multisection type reaction tower comprises at least four layers of conversion zone from top to bottom, and every layer of conversion zone is provided with column plate and forms bending runner and (namely set up hydraulic barrier, avoid possible Biased flow phenomenon, add the material time of staying on a catalyst), catalyst is filled with between column plate, also be provided with vapor riser (thus gas phase is communicated with) between the conversion zone of adjacent two layers, reaction tower tower top is also provided with gaseous phase outlet; Every layer of conversion zone is equipped with import and the outlet of band valve.
The products export of described separation of products tower is also connected with refining rectifying column (vacuum rectification tower), and this refining rectifying column also comprises the target product outlet that the heavy constituent be located at the bottom of tower exported, was located at tower top, and the pipeline of this target product outlet is provided with condenser.
The present invention with pure formaldehyde gas and dimethoxym ethane for raw material, high-temperature anhydrous formaldehyde gas and 90%--99% concentration dimethoxym ethane enter from the bottom of filler reaction tower and top respectively, formaldehyde gas is after bubble absorption, unabsorbed part rises through packing material absorbing section, now sprays fresh dimethoxym ethane solution and the dimethoxym ethane containing formaldehyde gas from column bottoms pump in spray system.And the first half of packing material absorbing section in tower is equipped with catalyst, spray and lower formalin and the formaldehyde gas do not absorbed completely absorb further in packing section, and carry out catalytic reaction generation polymethoxy dimethyl ether, now the operating temperature of filler reaction tower is 40 ~ 100 DEG C, pressure is normal pressure-0.5MPa, the formic acid that lower reaction temperature can suppress the disproportionated reaction of formaldehyde to generate, thus the conversion ratio of formaldehyde can be improved, promote the forward reaction of polymethoxy dimethyl ether.From the initial reaction of filler reaction tower, obtain the I order reaction liquid at the bottom of tower, component comprises formaldehyde 5-30%, and DMM1 contains 10-20% containing 40-60%, DMM3-8.Tower top withdraws the heat that reaction heat, absorption heat and formaldehyde self bring.Multistage reactor of the present invention adopts four sections of shunting means, and liquid phase can by Valve controlling, realizes series-parallelly freely changing, and gas phase is come round, and the dimethoxym ethane making it possible to volatilize, to tower top, takes away heat of reaction, and what promote to balance moves to right.Therefore, the series connection that multistage reactor four sections can be realized between any two by valve opening and closing uses.Effectively control the inversion equilibrium point of reaction, especially in catalyst activity changes, realize utilizing catalysis efficiently.
With pure formaldehyde gas and dimethoxym ethane for raw material, high-temperature anhydrous formaldehyde gas and 90%--99% concentration dimethoxym ethane enter from the bottom of filler reaction tower and top respectively, formaldehyde gas is after bubble absorption, unabsorbed part rises through packing material absorbing section, now sprays fresh dimethoxym ethane solution and the dimethoxym ethane containing formaldehyde gas from column bottoms pump in spray system.And the first half of packing material absorbing section in tower is equipped with catalyst, spray and lower formalin and the formaldehyde gas do not absorbed completely absorb further in packing section, and carry out catalytic reaction generation polymethoxy dimethyl ether, now the operating temperature of filler reaction tower is 40 ~ 100 DEG C, pressure is normal pressure-0.5MPa, the formic acid that lower reaction temperature can suppress the disproportionated reaction of formaldehyde to generate, thus the conversion ratio of formaldehyde can be improved, promote the forward reaction of polymethoxy dimethyl ether.The methyl alcohol that in reaction system, formic acid also carries with dimethoxym ethane in addition carries out esterification, and gone out with the form fractionation of gas methyl formate by the tower top of filler reaction tower, thus can avoid formic acid content in the accumulation maintenance system of formic acid a lower content under, realize the catalytic distillation mode that production limit, limit is separated.And the formic acid of the poly/trimerization/formalin adopted in commonsense method is too many, the forward reaction of polymethoxy dimethyl ether cannot be maintained by means of only the mode of methyl formate shifts out formic acid, along with the formic acid content that carries out of reaction increases gradually and causes the conversion ratio of reaction to reduce rapidly, therefore the way of alkali neutralization or adsorption deacidification can only be adopted to remove formic acid, just cause the problem of environmental pollution and waste of raw materials.
I order reaction liquid enters separation of products tower, the product of extraction DMM3-8 at the bottom of tower, and in the middle part of tower, extraction does not meet the light component of product requirement, and this light component comprises the DMM1 not participating in completely reacting, formaldehyde, methyl alcohol and reaction intermediate species DMM2.This part light component, after again preparing burden with dimethoxym ethane, enters 4 grades of multisection type reactors.II order reaction fluid component comprises formaldehyde 5-15%, and DMM1 contains 20-40% containing 30-50%, DMM3-8.II order reaction liquid pump enters separation of products tower, takes out the semi-finished product of DMM3-8, and it is refining it to be reduced pressure in refining rectifying column, obtains the product of the DMM3-5 being more applicable to doing diesel fuel additives.The composition of the DMMn > 5 that component is relatively heavier returns multistage reactor, and the effective molecular balance that stops, to the carrying out in larger polymer direction, improves conversion ratio and selective.Solve the uppity problem of fixed bed reaction actuator temperature, effectively raise the degree of reacting and carrying out.
Simultaneously, from the extraction of filler reaction tower containing the dimethoxym ethane gas of methyl formate first through condensation, highly purified methyl formate is isolated as accessory substance in the mode through compression rectification, and the dimethoxym ethane of separation at the bottom of tower then returns to filler reaction tower and continues reaction, methyl formate recovery tower operating temperature 40 DEG C-100 DEG C, pressure is normal pressure-0.8MPa.
Claims (5)
1. the multisection type reaction tower for polymethoxy dimethyl ether synthesis, it is characterized in that: described reaction tower tower body comprises at least two-layer conversion zone from top to bottom, and every layer of conversion zone is provided with column plate and forms bending runner, catalyst is filled with between column plate, also be provided with vapor riser between the conversion zone of adjacent two layers, reaction tower tower top is also provided with gaseous phase outlet; Every layer of conversion zone is equipped with import and the outlet of band valve.
2. multisection type reaction tower according to claim 1, is characterized in that: described conversion zone has four layers.
3. a process unit for gas formaldehyde synthesis polymethoxy dimethyl ether, is characterized in that: comprise filler reaction tower, separation of products tower and multisection type reaction tower, wherein:
Described filler reaction tower is provided with the packing section being filled with catalyst, spray system and bubble absorption section respectively above and below packing section, described filler reaction tower be also provided with the dimethoxym ethane entrance be connected with spray system, the formaldehyde gas entrance be connected with bubble absorption section, bottom first order reaction liquid export and the gaseous phase outlet at top; Described bubble absorption section is also communicated with dimethoxym ethane entrance by tubing pump;
The bottom first order reaction liquid outlet of described filler reaction tower is connected with the entrance of separation of products tower, described separation of products tower also comprises the products export, the gaseous phase outlet of tower top and the light fraction outlet on tower top that are located at the bottom of tower, the light fraction outlet on described tower top is connected by the import of pipeline with multisection type reaction tower, and this passage is also provided with dimethoxym ethane supply pipe; And the outlet of multisection type reaction tower is communicated with by the entrance of pipeline with separation of products tower.
4. process unit according to claim 3, it is characterized in that: the products export of described separation of products tower is also connected with refining rectifying column, this refining rectifying column also comprises the target product outlet that the heavy constituent be located at the bottom of tower exported, was located at tower top, and the pipeline of this target product outlet is provided with condenser.
5. process unit according to claim 3, is characterized in that: the gaseous phase outlet of described separation of products top of tower is communicated with the formaldehyde gas entrance of filler reaction tower by pipeline.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601479A (en) * | 2016-02-03 | 2016-05-25 | 陕西恒华能源科技有限公司 | Preparation method of polymethoxy dimethyl ether |
| CN105693479A (en) * | 2016-03-15 | 2016-06-22 | 江苏凯茂石化科技有限公司 | Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas |
| CN107285999A (en) * | 2017-07-13 | 2017-10-24 | 湖北三里枫香科技有限公司 | A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method |
| CN107445808A (en) * | 2017-09-08 | 2017-12-08 | 青岛迈特达新材料有限公司 | A kind of technique and system for preparing polymethoxy dimethyl ether |
| CN107522601A (en) * | 2017-09-08 | 2017-12-29 | 青岛迈特达新材料有限公司 | A kind of polymethoxy dimethyl ether separator and technique |
| CN107721831A (en) * | 2017-11-08 | 2018-02-23 | 江苏道尔顿石化科技有限公司 | A kind of polymethoxy dimethyl ether synthesizes the plug-in reaction system of bubble type and synthetic method |
| CN109232202A (en) * | 2018-11-08 | 2019-01-18 | 凯瑞环保科技股份有限公司 | A kind of one-step synthesis method DMM3-8Device and method |
| CN110078598A (en) * | 2019-04-16 | 2019-08-02 | 天津大学 | A kind of the multistage reactive distillation synthetic process and device of polymethoxy dimethyl ether |
| CN110090464A (en) * | 2019-04-16 | 2019-08-06 | 天津大学 | Partition wall reactive distillation method and device for polymethoxy dimethyl ether synthesis |
| CN110156575A (en) * | 2019-04-17 | 2019-08-23 | 天津大学 | Reactive distillation-Steam soak coupling technique for polymethoxy dimethyl ether synthesis |
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