CN103896747A - Backpack type circulation production process device of high-concentration methylal - Google Patents
Backpack type circulation production process device of high-concentration methylal Download PDFInfo
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- CN103896747A CN103896747A CN201410139249.0A CN201410139249A CN103896747A CN 103896747 A CN103896747 A CN 103896747A CN 201410139249 A CN201410139249 A CN 201410139249A CN 103896747 A CN103896747 A CN 103896747A
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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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- 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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a backpack type circulation production process device of high-concentration methylal. The process method comprises the step of dividing a one-tower process of reaction and distillation into two-tower processes of reaction and distillation, and can be used for effectively improving the conversion rate of methylal and obtaining more than 99.5% of high-concentration methylal while greatly lowering the height of a reactive distillation tower in the prior art so as to reduce the investment; moreover, the process also reduces the wastewater discharge and heat energy consumption by adopting a plurality of reflux circulations and surplus heat sources.
Description
Technical field
The present invention relates to methylal production technical field, relate in particular to the production technology that concentration is more than 99.9% high-concentration methylal.
Background technology
Methylal has good physicochemical property, be good solubility, lower boiling, good with water dissolubility, can be widely used in the products such as makeup, medicine, household supplies, industrial Automobile Products, sterilant, leather polish, sanitising agent, rubber industry, paint, ink, also because methylal (109-87-5) has good ability of cleaning greasy dirt and volatility, can substitute F11 and F113 and chlorinated solvents as sanitising agent, therefore be replacement fluorine Lyons, reduce volatile organic matter (VOCs) discharge, reduce the environmentfriendly products to topsoil.Development in recent years is very fast, has especially represented good application development prospect in aerosol field.
Current domestic high-concentration methylal has two kinds of techniques, and one is extraction process, and the methylal technique of extraction needs solvent, and the loss of solvent pollutes, and the recovery of solvent simultaneously needs energy consumption, causes product energy consumption high, complex process.Another kind is compression rectification, and the production process equipment investment of the methylal of compression rectification method is originally larger, and methylal waste water COD content is larger, more difficult, causes product cost high.
Summary of the invention
Goal of the invention: for problem and the defect of above-mentioned existence, the invention provides a kind of high-concentration methylal Backpack type cycle production process device and method, flow process is simpler, less investment, waste water content is low, by product is few and energy consumption is low advantage.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of high-concentration methylal Backpack type cycle production process device, comprise pre-reactor, reactive distillation column, rectifying tower, pressure distillation tower, Backpack type reactor, reboiler, evaporative condenser and return tank, described reactive distillation column, the bottom of rectifying tower and pressure distillation tower is equipped with reboiler, described reactive distillation column comprises rectifying section and is located at the conversion zone on top, conversion zone is the multilayered structure being communicated with up and down, every layer is all connected to form circulation by pipeline and single Backpack type reactor, the outlet of described pre-reactor is connected with the entrance of reactive distillation column by pipeline, the pipeline that passes through of reactive distillation column overhead is connected with rectifying tower entrance, rectifying tower tower top connects evaporative condenser and return tank successively, and return tank is connected with pressure distillation tower by pipeline again, at the bottom of the tower of described reactive distillation column, be provided with wastewater outlet, at the bottom of the tower of described rectifying tower, be connected to form reflux cycle by the tower top of pipeline and reactive distillation column, the tower top circulation that described return tank is also provided with branch road and rectifying tower is connected, and the tower top of described pressure distillation tower is by pipeline and the supporting reboiler formation heat exchange circulation passage of reactive distillation column simultaneously.
As preferably, at the bottom of the tower of described pressure distillation tower, be also connected with adsorption tanks and products pot in turn by pipeline.
As preferably, described Backpack type reactor is 8, and with the relatively independent setting of reactive distillation column.
As preferably, described pre-reactor is the fixed bed catalyst reactor of two series connection, and is furnished with the fixed bed catalyst reactor of adapted.
As preferably, described pressure distillation column overhead is undertaken after heat exchange by pipeline and the supporting reboiler of reactive distillation column, then is connected with pressure distillation tower and rectifying tower respectively by pipeline.
Beneficial effect: compared with prior art, the present invention has the following advantages: change two tower process into by an original tower process, can reduce the height of tower, greatly reduce facility investment; 8 reactors of reactive distillation column, can make the not formaldehyde in pre-reactor complete reaction, methyl alcohol continue reaction, until complete reaction.Make the waste water COD≤30ppm at the bottom of reactive distillation column, directly reach emission standard; Methylal plate-type condenser is changed as energy-conservation evaporative condenser, and high without heat exchange efficiency, the investment of also having saved the floor space of circulating water pool and pipeline, pump, and the consumption of saving power consumption and water, reduce production costs.
Accompanying drawing explanation
Fig. 1 is the technological process of production schematic diagram of described high-concentration methylal of the present invention.
Wherein, pre-reactor 1, reactive distillation column 2, Backpack type reactor 3, rectifying tower 4, evaporative condenser 5, return line 6, pressure distillation tower 7, reboiler 8.
Embodiment
Below in conjunction with the drawings and specific embodiments, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
As shown in Figure 1, a kind of technological process of production of high-concentration methylal, after raw material formaldehyde and methanol mixed, send into pre-reactor, methylal, water and the formaldehyde not reacted, the reacted solution of methyl alcohol that generate through reaction enter after reactive distillation column, in conversion zone, responseless formaldehyde and methyl alcohol are sent in 8 Backpack type reactors by reactor pump circulation, after reaction in Backpack type reaction after recycled back reactive distillation column.Successively after 8 side reactors, through reactive distillation, methylal is gone out to enter follow-up rectifying tower from reactive distillation column overhead with methyl alcohol and is further separated, the water that reacted water and methylal generate from sending at the bottom of tower after surge tank buffering after pump extraction, send into evaporative condenser through overcooling again, as the make up water of evaporative condenser, thus can water saving.Methylal in rectifying tower and methyl alcohol process separate, the water at the bottom of rectifying tower, methylal, methyl alcohol backflow as reactive distillation column through reflux pump; 92% methylal enters return tank from rectifying tower tower top after evaporative condenser condensation.A part is as the backflow of rectifying tower, and a part enters pressure distillation tower, in pressurizing tower methylal and methyl alcohol through separation, 99.5% methylal from the bottom of tower as product extraction.The methylal of pressurizing tower tower top and methyl alcohol are as the thermal source reboiler heating of reactive distillation column, and condensation rear portion goes pressurizing tower to reflux, and a part is gone rectifying tower rectifying.
Because this process using solid acid is as catalyzer, reaction and rectifying are separated, not at a chemical industry equipment device, can reduce like this height of equipment, reduce investment outlay; 8 reactors of simultaneous reactions rectifying tower, can more fully react methyl alcohol and formaldehyde, and the COD content of waste water is low, reaches emission standard.The gas of pressurizing tower, as the thermal source of reactive distillation column, replaces steam heating, makes heat recovery and utilization.And the cost of product.Following table is the contrast of processing method of the present invention and prior art.Therefore this technique is passed through a tower process of just reaction and rectifying, be divided into two tower process of reaction and rectifying, when the turnover ratio that can effectively improve methylal obtains exceeding 99.5% high-concentration methylal, the height of the reactive distillation column of prior art is reduced greatly, thereby reduced investment; In addition, this technique also adopts multiple reflux cycle and thermal source more than needed, has reduced discharge of wastewater and heat energy consumption.
Starting material and power consumption contrast (in per ton 99.5%) in each technique
Claims (5)
1. a high-concentration methylal Backpack type cycle production process device, it is characterized in that: comprise pre-reactor, reactive distillation column, rectifying tower, pressure distillation tower, Backpack type reactor, reboiler, evaporative condenser and return tank, the bottom of described reactive distillation column, rectifying tower and pressure distillation tower is equipped with reboiler, described reactive distillation column comprises rectifying section and is located at the conversion zone on top, conversion zone is the multilayered structure being communicated with up and down, and every layer is all connected to form circulation by pipeline and single Backpack type reactor; The outlet of described pre-reactor is connected with the entrance of reactive distillation column by pipeline, the pipeline that passes through of reactive distillation column overhead is connected with rectifying tower entrance, rectifying tower tower top connects evaporative condenser and return tank successively, and return tank is connected with pressure distillation tower by pipeline again; At the bottom of the tower of described reactive distillation column, be provided with wastewater outlet, at the bottom of the tower of described rectifying tower, be connected to form reflux cycle by the tower top of pipeline and reactive distillation column, the tower top circulation that described return tank is also provided with branch road and rectifying tower is connected, and the tower top of described pressure distillation tower is by pipeline and the supporting reboiler formation heat exchange circulation passage of reactive distillation column simultaneously.
2. high-concentration methylal Backpack type cycle production process device according to claim 1, is characterized in that: at the bottom of the tower of described pressure distillation tower, be also connected with adsorption tanks and products pot in turn by pipeline.
3. high-concentration methylal Backpack type cycle production process device according to claim 1, is characterized in that: described Backpack type reactor is 8, and with the relatively independent setting of reactive distillation column.
4. high-concentration methylal Backpack type cycle production process device according to claim 1, is characterized in that: described pre-reactor is the fixed bed catalyst reactor of two series connection, and is furnished with the fixed bed catalyst reactor of adapted.
5. high-concentration methylal Backpack type cycle production process device according to claim 1, it is characterized in that: described pressure distillation column overhead is undertaken after heat exchange by pipeline and the supporting reboiler of reactive distillation column, then is connected with pressure distillation tower and rectifying tower respectively by pipeline.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410139249.0A CN103896747A (en) | 2014-04-08 | 2014-04-08 | Backpack type circulation production process device of high-concentration methylal |
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| CN201410139249.0A CN103896747A (en) | 2014-04-08 | 2014-04-08 | Backpack type circulation production process device of high-concentration methylal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254478A (en) * | 2015-09-28 | 2016-01-20 | 常州工程职业技术学院 | Production technology for homogeneous catalytic synthesis of methylal |
| CN107986947A (en) * | 2017-12-28 | 2018-05-04 | 四川鑫达新能源科技有限公司 | A kind of dimethoxym ethane heat integration synthesis system and preparation method |
| CN113214055A (en) * | 2021-05-19 | 2021-08-06 | 宁夏华业精细化学科技有限公司 | Methylal production process |
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| US7534922B2 (en) * | 2004-12-13 | 2009-05-19 | Ticona Gmbh | Processes for the manufacture of acetals |
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| CN101857534A (en) * | 2010-06-03 | 2010-10-13 | 濮阳市普天化工有限公司 | Technique for synthesizing methylal |
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| CN204162632U (en) * | 2014-04-08 | 2015-02-18 | 江苏凯茂石化科技有限公司 | A kind of high-concentration methylal Backpack type cycle production process device |
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2014
- 2014-04-08 CN CN201410139249.0A patent/CN103896747A/en active Pending
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| US7534922B2 (en) * | 2004-12-13 | 2009-05-19 | Ticona Gmbh | Processes for the manufacture of acetals |
| CN101786946A (en) * | 2010-04-01 | 2010-07-28 | 江苏恒茂机械制造有限公司 | Methylal preparation device |
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| CN101857534A (en) * | 2010-06-03 | 2010-10-13 | 濮阳市普天化工有限公司 | Technique for synthesizing methylal |
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| CN103657130A (en) * | 2013-12-03 | 2014-03-26 | 惠州市利而安化工有限公司 | External-arrangement reactor type methylal rectifying tower |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254478A (en) * | 2015-09-28 | 2016-01-20 | 常州工程职业技术学院 | Production technology for homogeneous catalytic synthesis of methylal |
| CN107986947A (en) * | 2017-12-28 | 2018-05-04 | 四川鑫达新能源科技有限公司 | A kind of dimethoxym ethane heat integration synthesis system and preparation method |
| CN113214055A (en) * | 2021-05-19 | 2021-08-06 | 宁夏华业精细化学科技有限公司 | Methylal production process |
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Application publication date: 20140702 |