CN111233640B - Production process and device of high-purity methylal - Google Patents
Production process and device of high-purity methylal Download PDFInfo
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Abstract
The invention discloses a production process of high-purity methylal, belonging to the technical field of methylal production and comprising the following steps: mixing methanol and a formaldehyde solution, and then, reacting in a reactive distillation tower to obtain an azeotropic mixture of methylal and methanol; the catalyst in the reactive distillation column is strong acid cation exchange resin, and the resin is modularly installed in the reactive distillation column; the azeotropic mixture enters a pressurized rectifying tower for separation, and a separation product at the bottom of the pressurized rectifying tower is condensed to obtain a product; a mixture of methylal and methanol is obtained from the top of the pressurized rectifying tower, and part of the mixture enters a catalyst layer at the lower part of the reactive rectifying tower and continues to participate in the reaction; the method adopts a double tower of the reaction rectifying tower and the pressurization rectifying tower, the obtained product has high quality, the purity of the methylal product is more than 99.9 percent, the moisture content is less than 0.03 percent, and the product quality is obviously improved; the waste water is easy to treat, the energy consumption of production is reduced, and the equipment investment is small.
Description
Technical Field
The invention relates to the technical field of methylal production, in particular to a synthesis process and a synthesis device of high-purity methylal.
Background
The methylal is prepared by condensation reaction of methanol and formaldehyde solution as raw materials and rectification purification, and is widely applied to products such as cosmetics, medicines, industrial and automobile products, insecticides, leather polishing agents, cleaning agents, rubber industry, paints, printing ink and the like.
There have been many reports on the production process of methylal. Because methylal obtained after the reaction of methanol and formaldehyde contains impurities such as methanol, formaldehyde and the like, various alcohols and derivatives thereof are generally added for extraction, rectification and purification in the prior art, and although the methods can greatly improve the purity of methylal, such as 98.5 percent or even more than 99 percent, various extracting agents are needed, on one hand, new impurities are introduced, and on the other hand, environmental protection is also influenced.
In order to solve the above problems, chinese patent application No. 201010250317.2, patent name: the patent of high-concentration methylal pressure distillation process and preparation device discloses a production method of high-purity methylal by adopting a reaction distillation column and a differential pressure distillation column, which solves the problems of adding various extracting agents, but still has the following problems:
1. a pre-reactor still needs to be arranged, so that the equipment investment and the equipment floor area are large; 2. although the patent document does not disclose the purity data of the obtained methylal, the inventor of the application adopts the method to prepare the methylal in the test process, and the purity of the obtained methylal is 98.21 percent, the methanol content is 1.73 percent, and the purity of the methylal is further improved; in addition, the water content of the obtained methylal is 0.06 percent, the water content is higher, the quality of the methylal product is influenced, in addition, the formaldehyde content in the wastewater at the bottom of the reactive distillation tower is 3.3 percent, the methanol content is 0.19 percent, and the difficulty of wastewater treatment is increased.
Disclosure of Invention
One of the objectives of the present invention is to provide a process for producing high purity methylal, so as to solve the above problems.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a production process of high-purity methylal comprises the following steps:
(1) Mixing methanol and a formaldehyde solution, and then, reacting in a reactive distillation tower to obtain an azeotropic mixture of methylal and methanol; the catalyst in the reactive distillation column is strong acid cation exchange resin, and the strong acid cation exchange resin is modularly installed in the reactive distillation column;
(2) Feeding the methylal and methanol azeotropic mixture obtained in the step (1) into a pressurized rectifying tower for separation, and condensing a separation product at the bottom of the pressurized rectifying tower to obtain methylal with the purity of more than 99.9%; and (3) obtaining a mixture of methylal and methanol at the top of the pressurized rectifying tower, wherein one part of the mixture enters a catalyst layer at the lower part of the reactive rectifying tower in the step (1) and continuously participates in the reaction.
As a preferred technical scheme: in the step (1), the feed concentration of the formaldehyde is 30-60%; the mass ratio of the methanol to the formaldehyde is 1.1: 1-2.0: 1 (the mass ratio is calculated by the mass of the pure methanol and the pure formaldehyde, and the relative excess of the methanol is ensured); the reaction temperature of the reaction rectifying tower is 50-85 ℃. The raw materials of the process have wider adaptability to the concentration of the formaldehyde raw materials, 30-60% of formaldehyde solution can meet the requirements of the process, and high-purity methylal products are produced.
As a preferred technical scheme: in the step (1), the modular installation mode of the catalyst is as follows: the thickness of each catalyst module is 10-20 cm, the filling amount of each catalyst section is 10-15 layers, the number of catalysts in the reaction section is not less than three, the number of catalysts in the rectification section is not less than two, the distance between the sections is 20-40 cm, and the total filling section of the catalysts is not less than five.
As a further preferable technical scheme: in the step (1), the modular installation mode of the catalyst is as follows: the thickness of each catalyst module is 12-18 cm, the filling amount of each catalyst section is 11-14 layers, the catalyst of the reaction section is not less than three sections, the catalyst of the rectification section is not less than two sections, the distance between each section is 25-35 cm, and the total filling section of the catalyst is not less than five sections.
As a preferred technical scheme: in the step (2), the operating pressure of the pressurized rectifying tower is 1.0-2.0 Mpa.
As a further preferable technical scheme: in the step (2), the operating pressure of the pressurized rectifying tower is 1.2-1.6 Mpa.
As a preferred technical scheme: in the step (2), the temperature of the top of the pressurized rectifying tower is 100-130 ℃, and the temperature of the bottom of the tower is 120-140 ℃.
For the further preferred technical scheme: in the step (2), the tower top temperature of the pressurized rectifying tower is 110-125 ℃, and the tower kettle temperature is 125-135 ℃.
As a preferred technical scheme: in the step (2), the gas-phase component distilled from the top of the pressurized rectifying tower is used as one of the heat sources at the bottom of the reactive rectifying tower. The energy consumption can be reduced by more than 30%.
As a preferred technical scheme: in the step (2), the gas-phase component distilled from the top of the pressurized rectifying tower enters the lower part of the catalyst layer of the reactive rectifying tower. The gas phase components distilled from the top of the pressurized rectifying tower are methanol and methylal, and enter the lower part of the catalyst layer of the reactive rectifying tower, wherein the methanol can fully react with material formaldehyde, so that the formaldehyde can completely react, the utilization rate of the material is improved, the formaldehyde content in the wastewater at the bottom of the tower is reduced, and the formaldehyde content is less than 500PPM.
The process conditions of the invention can be summarized as follows: mixing an industrial methanol raw material with the purity of more than 99.5 percent and a 30-60 percent formaldehyde solution by a static feeding mixer, then exchanging heat with wastewater from the bottom of a reaction rectifying tower by a tubular heat exchanger, and then entering the reaction rectifying tower from the middle upper part of the reaction rectifying tower, wherein the temperature of a reaction section is 50-85 ℃, and the temperature of the top of the reaction rectifying tower is 35-45 ℃; the composition of the methylal crude product obtained from the tower top is 88 to 92 percent of methylal, 8 to 14 percent of methanol and 0 to 0.05 percent of water, and the mixture enters a pressurized rectifying tower; the content of formaldehyde in the wastewater obtained from the bottom of the reactive distillation tower is 10-500 PPM and methanol is not contained.
In traditional methylal production process, the top of the reactive distillation tower wants to obtain methylal with higher purity, then the content of formaldehyde in wastewater at the bottom of the tower is higher, namely the higher purity methylal intermediate product and the lower content of formaldehyde in wastewater can not be taken into consideration, and the application can not only improve the conversion rate of formaldehyde but also reduce the content of formaldehyde in wastewater at the bottom of the reactive distillation tower by reducing the content of formaldehyde below 500pp through arranging a special catalyst layer structure on one hand, and on the other hand, introduce a mixture at the top of the pressurized distillation tower into a catalyst layer at the lower part of the reactive distillation tower for reaction, thereby solving the problem that the two products can not be taken into consideration, and simultaneously, the purity of the methylal obtained at the top of the tower can reach more than 90 percent, thereby providing guarantee for obtaining higher purity methylal products subsequently.
The operating pressure of the pressurized rectifying tower is 1.0-1.2 Mpa, the temperature of the tower top is 100-130 ℃, and the temperature of the tower kettle is 120-140 ℃; a methylal product with more than 99.9 percent and water content less than 0.03 percent is obtained at the bottom of the pressurized rectifying tower, a mixture of methylal, methanol and water obtained at the top of the tower enters the reactive rectifying tower for heat energy utilization, then enters a reflux tank of the rectifying tower, one part of the mixture enters the pressurized rectifying tower as reflux, and the other part of the mixture enters a lower catalyst layer of the reactive rectifying tower to continuously participate in the reaction for cyclic utilization;
as a preferred technical scheme: in the step (1), the waste water at the bottom of the reactive distillation tower exchanges heat with the feed. The heat of the wastewater at the bottom of the reaction rectifying tower can be utilized to improve the feeding problem, and the energy is saved.
The second purpose of the present invention is to provide a production apparatus used in the above production process, which comprises a raw material mixer and a reactive distillation column, wherein the raw material mixer is connected with the middle part of the reactive distillation column, a catalyst layer is arranged on the lower part in the reactive distillation column, the top of the reactive distillation column is sequentially connected with a first condenser, a first reflux tank and a pressurized distillation column, and the apparatus further comprises a second reflux tank, the first reflux tank is connected with the middle part of the pressurized distillation column, the top of the pressurized distillation column is respectively connected with the catalyst layer on the lower part of the reactive distillation column and the second reflux tank, and the second reflux tank is further connected with the pressurized distillation column.
As a preferred technical scheme: the catalyst of the catalyst layer is installed in a modularization mode.
Compared with the prior art, the invention has the advantages that: the invention adopts a double-tower process of a reaction rectifying tower and a pressurized rectifying tower, the purity of the obtained methylal product is more than 99.9 percent, the moisture content is less than 0.03 percent, and the product quality is obviously improved; the content of formaldehyde in the generated wastewater is less than 500PPM, methanol is not contained, and the wastewater is easy to treat; the invention utilizes the heat of the waste water at the bottom of the reactive distillation tower and the heat of the top of the pressurizing distillation tower, thereby reducing the energy consumption of production; the invention has simple process, no need of pre-reactor and low equipment investment.
Drawings
FIG. 1 is a schematic view of a production apparatus of the present invention;
in the figure: 1. a formaldehyde tank; 2. a methanol tank; 3. a raw material mixer; 4. a heat exchanger; 5. a reactive distillation column; 51. a catalyst layer; 6. a pressurized rectifying tower; 71. a first condenser; 72. a second condenser; 73. a third condenser; 81. a first reflux drum; 82. a second reflux drum; 91. a first pump; 92. a second pump; 93. a third pump; 94. a fourth pump; 95 a fifth pump; 96. and a sixth pump.
Detailed Description
The invention will be further explained with reference to the drawings.
Example 1:
referring to fig. 1, a high-purity methylal production device comprises a formaldehyde tank 1, a methanol tank 2, a raw material mixer 3 and a reactive distillation column 5, wherein a first pump 91 is arranged between the formaldehyde tank 1 and the raw material mixer 3, a second pump 92 is arranged between the methanol tank 2 and the raw material mixer 3, a tubular heat exchanger 4 is arranged between the raw material mixer 3 and the reactive distillation column 5, the heat exchanger 4 is connected with the middle part of the reactive distillation column 5, a catalyst layer 51 is arranged at the lower part in the reactive distillation column 5, the top of the reactive distillation column 5 is sequentially connected with a first condenser 71, a first reflux tank 81 and a pressurized distillation column 6, the high-purity methylal production device further comprises a second reflux tank 82, a fourth pump 94 is arranged between the first reflux tank 81 and the pressurized distillation column 6, the fourth pump 94 is connected with the middle part of the pressurized distillation column 6, the top of the pressurized distillation column 6 is connected with a second condenser 72, the second condenser 72 is respectively connected with the catalyst layer 51 at the lower part of the reactive distillation column 5 and the second reflux tank 82, the second reflux tank 82 is connected with a fifth reflux pump 95, and the pressurized distillation column 6;
the tower bottom of the reaction rectifying tower 5 is provided with a third pump 93, and the third pump 93 is connected with the heat exchanger 4; a sixth pump 96 and a third condenser 73 are sequentially arranged at the bottom of the pressurized rectifying tower 6;
the production method of the high-purity methylal by adopting the production device comprises the following steps:
the method comprises the following steps:
(1) Methanol and formaldehyde solution are respectively pumped into a raw material mixer 3 through a first pump 91 and a second pump 92 to be mixed, and then enter a reaction rectifying tower 5 through a tube type heat exchanger 4 to react, wherein the concentration of the raw material methanol is 99.5%, the concentration of the formaldehyde is 37.5%, the tower top temperature of the reaction rectifying tower is 38.5 ℃, the tower bottom temperature is 99.4 ℃, the reflux ratio is 1.5 times of the minimum reflux ratio, and an azeotropic mixture of methylal and methanol is obtained after the reaction, and the azeotropic mixture comprises the following components: 90.12% of methylal, 9.95% of methanol and 0.03% of water; the wastewater at the bottom of the reactive distillation tower comprises the following components: no methanol and formaldehyde 0.04%; the catalyst layer 51 in the reactive distillation column 5 is a strong acid cation exchange resin, the strong acid cation exchange resin is modularly installed in the reactive distillation column, and the specific filling mode is as follows: the thickness of each catalyst module is 15cm, the loading amount of each catalyst section is 12 layers, the total loading section of the catalyst is five sections, the catalyst of the reaction section is three sections, the catalyst of the rectification section is two sections, and the distance between the sections is 30cm;
(2) Enabling the methylal and methanol azeotropic mixture obtained in the step (1) to sequentially pass through a first condenser 71 and a first reflux tank 82 and enter the middle part of a pressurized rectifying tower 6 for separation, wherein the top temperature of the pressurized rectifying tower 6 is 135.2 ℃, the bottom temperature of the pressurized rectifying tower is 137.9 ℃, the reflux ratio is 1.7 times of the minimum reflux ratio, the top pressure of the pressurized rectifying tower is 1.18MPa, and a separation product at the bottom of the pressurized rectifying tower is condensed to obtain methylal with the purity of 99.93 percent, wherein the methanol content is 0.05 percent, and the water content is 0.02 percent; and (2) obtaining a mixture of methylal and methanol at the top of the pressurized rectifying tower, wherein the mixture consists of the methylal, the methanol and water, and one part of the mixture enters a catalyst layer at the lower part of the reactive rectifying tower in the step (1) to continuously participate in the reaction.
In the whole reaction process, 34 percent of energy can be saved.
Example 2:
(1) Methanol and formaldehyde solution are respectively pumped into a raw material mixer 3 through a first pump 91 and a second pump 92 to be mixed, and then enter a reaction rectifying tower 5 through a tubular heat exchanger 4 to react, wherein the concentration of the raw material methanol is 99.5%, the concentration of the formaldehyde is 31.2%, the top temperature of the reaction rectifying tower is 36.5 ℃, the bottom temperature of the reaction rectifying tower is 99.4 ℃, the reflux ratio is 1.8 times of the minimum reflux ratio, and an azeotropic mixture of methylal and methanol is obtained after the reaction, and the azeotropic mixture comprises: 88.93% of methylal, 11.03% of methanol and 0.04% of water; the wastewater at the bottom of the reactive distillation tower comprises the following components: no methanol and formaldehyde 0.04%; the catalyst layer 51 in the reactive distillation column 5 is a strong acid cation exchange resin, and the strong acid cation exchange resin is modularly installed in the reactive distillation column; the specific filling mode is as follows: the thickness of each catalyst module is 12cm, the loading amount of each catalyst section is 10 layers, the total loading sections of the catalyst are five sections, the catalyst of the reaction section is three sections, the catalyst of the rectification section is three sections, and the distance between the sections is 35cm;
(2) Enabling the methylal and methanol azeotropic mixture obtained in the step (1) to sequentially pass through a first condenser 71 and a first reflux tank 82 and enter the middle part of a pressurized rectifying tower 6 for separation, wherein the top temperature of the pressurized rectifying tower 6 is 126.5 ℃, the bottom temperature of the pressurized rectifying tower is 129.4 ℃, the reflux ratio is 1.5 times of the minimum reflux ratio, the top pressure of the pressurized rectifying tower is 1.12MPa, and a separation product at the bottom of the pressurized rectifying tower is condensed to obtain methylal with the purity of 99.91 percent, wherein the methanol content is 0.07 percent, and the water content is 0.02 percent; and (3) obtaining a mixture of methylal and methanol at the top of the pressurized rectifying tower, wherein the mixture consists of the methylal, the methanol and water, and part of the mixture enters a catalyst layer at the lower part of the reactive rectifying tower in the step (1) to continuously participate in the reaction.
Example 3:
(1) Methanol and formaldehyde solution are respectively pumped into a raw material mixer 3 through a first pump 91 and a second pump 92 to be mixed, and then enter a reaction rectifying tower 5 through a tubular heat exchanger 4 to react, wherein the concentration of the raw material methanol is 99.5%, the concentration of the formaldehyde is 56.5%, the top temperature of the reaction rectifying tower is 43.5 ℃, the bottom temperature of the reaction rectifying tower is 99.4 ℃, the reflux ratio is 1.6 times of the minimum reflux ratio, and an azeotropic mixture of methylal and methanol is obtained after the reaction, and the azeotropic mixture comprises the following components: 91.82% of methylal, 8.16% of methanol and 0.02% of water; the wastewater at the bottom of the reaction rectifying tower comprises the following components: no methanol and formaldehyde 0.02%; the catalyst layer 51 in the reactive distillation column 5 is a strong acid cation exchange resin, the strong acid cation exchange resin is modularly installed in the reactive distillation column, and the specific filling mode is as follows: the thickness of each catalyst module is 18cm, the loading of each catalyst section is 15 layers, the total loading section of the catalyst is seven sections, the catalyst of the reaction section is four sections, the catalyst of the rectification section is three sections, and the distance between the sections is 25cm;
(2) Enabling the methylal and methanol azeotropic mixture obtained in the step (1) to sequentially pass through a first condenser 71 and a first reflux tank 82 and enter the middle part of a pressurized rectifying tower 6 for separation, wherein the top temperature of the pressurized rectifying tower 6 is 130.2 ℃, the bottom temperature of the pressurized rectifying tower is 132.5 ℃, the reflux ratio is 1.6 times of the minimum reflux ratio, the top pressure of the pressurized rectifying tower is 1.15MPa, and a separation product at the bottom of the pressurized rectifying tower is condensed to obtain methylal with the purity of 99.94 percent, wherein the methanol content is 0.04 percent, and the water content is 0.02 percent; and (3) obtaining a mixture of methylal and methanol at the top of the pressurized rectifying tower, wherein the mixture consists of the methylal, the methanol and water, and part of the mixture enters a catalyst layer at the lower part of the reactive rectifying tower in the step (1) to continuously participate in the reaction.
Comparative example:
comparative example 1:
according to the process and the equipment of the embodiment 1, only the filling mode of the catalyst of the embodiment 1 is changed into a traditional fixed bed mode, the trend of materials is not changed, the operation parameters of the device are not changed, and the following effects are obtained:
the operation results of the reactive distillation column 5 are as follows:
the tower top material composition (mass percent): 90.32% of methylal, 8.52% of methanol and 1.16% of water;
the wastewater at the bottom of the tower comprises the following components in percentage by mass: 0.17% of methanol and 2.12% of formaldehyde;
the operation of the pressurized rectifying column 6 results as follows:
the tower bottom product comprises the following components in percentage by mass: 98.96% of methylal, 0.42% of methanol and 0.62% of water.
Comparative example 2:
according to the process and the equipment of the previous example 1 and the filling mode of the catalyst, only the direction of materials is changed: the tower top material of the pressurized rectifying tower 6 is changed to return to the raw material formaldehyde tank of the reactive rectifying tower, the rest operation parameters of the device are not changed, and the obtained effects are as follows:
the operation results of the reactive distillation column 5 are as follows:
azeotropic composition at the top of the column (mass): 90.31 percent of methylal, 8.54 percent of methanol and 1.15 percent of water.
The wastewater at the bottom of the tower comprises the following components (by mass): 0.06% of methanol and 3.02% of formaldehyde.
The operation of the pressurized rectifying column 6 results as follows:
the product at the bottom of the tower comprises the following components (by mass): 98.95% of methylal, 0.45% of methanol and 0.60% of water.
The comparison examples show that the technical contribution of the catalyst filling mode and the technical scheme of returning the materials at the top of the pressurized rectifying tower to the position of the reactive rectifying tower is very obvious to the technical contribution of improving the purity of the product and reducing the formaldehyde content of the wastewater.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (7)
1. A production process of high-purity methylal is characterized by comprising the following steps:
(1) Mixing methanol and a formaldehyde solution, and then, reacting in a reactive distillation tower to obtain an azeotropic mixture of methylal and methanol; the catalyst in the reactive distillation column is strong acid cation exchange resin, and the strong acid cation exchange resin is modularly installed in the reactive distillation column; the modular installation mode of the catalyst is as follows: the thickness of each catalyst module is 10-20 cm, the loading of each catalyst section is 10-15 layers, the catalyst of the reaction section is not less than three sections, the catalyst of the rectification section is not less than two sections, the distance between each section is 20-40 cm, and the total loading section of the catalyst is not less than five sections;
(2) Feeding the methylal and methanol azeotropic mixture obtained in the step (1) into a pressurized rectifying tower for separation, and condensing a separation product at the bottom of the pressurized rectifying tower to obtain methylal with the purity of more than 99.9%; and (3) obtaining a mixture of methylal and methanol at the top of the pressurized rectifying tower, wherein one part of the mixture enters a catalyst layer at the lower part of the reactive rectifying tower in the step (1) and continuously participates in the reaction.
2. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: in the step (1), the feed concentration of the formaldehyde is 30-60%; the mass ratio of the methanol to the formaldehyde is 1.1: 1-2.0: 1; the reaction temperature of the reaction rectifying tower is 50-85 ℃.
3. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: in the step (2), the operating pressure of the pressurized rectifying tower is 1.0-2.0 Mpa.
4. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: in the step (2), the temperature of the top of the pressurized rectifying tower is 100-130 ℃, and the temperature of the bottom of the tower is 120-140 ℃.
5. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: in the step (2), the gas-phase component distilled from the top of the pressurized rectifying tower is used as one of the heat sources at the bottom of the reactive rectifying tower.
6. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: in the step (2), the gas-phase component distilled from the top of the pressurized rectifying tower enters the lower part of the catalyst layer of the reactive rectifying tower.
7. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: in the step (1), the waste water at the bottom of the reactive distillation tower exchanges heat with the feed.
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| CN102557898A (en) * | 2010-12-20 | 2012-07-11 | 天津天大天久科技股份有限公司 | Method and device for preparing high-concentration methylal |
| CN102070417A (en) * | 2011-01-06 | 2011-05-25 | 福州大学 | Dimethoxym ethane catalytic distillation production process and production equipment thereof |
| CN102417442A (en) * | 2011-10-25 | 2012-04-18 | 中国海洋石油总公司 | Preparation method for high-purity methylal |
| CN103936569B (en) * | 2014-04-08 | 2016-03-30 | 江苏凯茂石化科技有限公司 | A kind of high-concentration methylal production technique apparatus and method |
| CN104447240A (en) * | 2014-11-10 | 2015-03-25 | 中国海洋石油总公司 | Method for preparing high-purity methylal |
| CN205886901U (en) * | 2016-03-14 | 2017-01-18 | 凯瑞环保科技股份有限公司 | Module catalyst that gathers methoxy dimethyl ether with bed technique production of full room |
| CN208717197U (en) * | 2018-05-22 | 2019-04-09 | 凯瑞环保科技股份有限公司 | A kind of device producing high-purity dimethoxym ethane using catalytic distillation coupling technique |
| CN108424358B (en) * | 2018-05-22 | 2023-12-26 | 凯瑞环保科技股份有限公司 | Device and method for producing high-purity methylal by utilizing catalytic distillation coupling technology |
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