CN112266324B - Method and device for preparing methyl methacrylate by continuously regenerating waste acrylic - Google Patents
Method and device for preparing methyl methacrylate by continuously regenerating waste acrylic Download PDFInfo
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- CN112266324B CN112266324B CN202011165312.XA CN202011165312A CN112266324B CN 112266324 B CN112266324 B CN 112266324B CN 202011165312 A CN202011165312 A CN 202011165312A CN 112266324 B CN112266324 B CN 112266324B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention belongs to the technical field of acrylic recovery, and relates to a method for preparing methyl methacrylate by continuously regenerating waste acrylic, which comprises the following steps: crushing the waste acrylic; sequentially degrading acrylic granules through a melting zone, a first-order degradation zone and a second-order degradation zone of a degradation unit to generate methyl methacrylate gas, wherein the melting zone, the first-order degradation zone and the second-order degradation zone are controlled by adopting multi-section temperature, the temperature of the melting zone is controlled to be 200-270 ℃ and is increased section by section, the temperature of the first-order degradation zone is controlled to be 280-400 ℃ and is increased section by section, and the temperature of the second-order degradation zone is controlled to be 380-150 ℃ and is reduced section by section; rectifying and purifying the methyl methacrylate gas to obtain a methyl methacrylate finished product. The invention also provides a device using the method. The method and the device for preparing the methyl methacrylate by continuously regenerating the waste acrylic improve the degradation conversion rate, and the process is more closed, continuous and automatic.
Description
Technical Field
The invention belongs to the technical field of acrylic recovery, and relates to a method and a device for preparing methyl methacrylate by continuously regenerating waste acrylic.
Background
Acrylic (PMMA), the chemical name of which is polymethyl methacrylate, is obtained from the free radical polymerization of Methyl Methacrylate (MMA) monomers, and is an important thermoplastic. The waste acrylic is from industrial waste materials such as leftover materials and cutting scraps in machining, and organic glass plates, engineering plastics and civil consumer goods after being used can save resources and protect the environment if the waste materials can be effectively recycled, and good economic benefits can be formed by fully utilizing recycled products.
The degradation methods adopted in industry are: dry distillation, superheated steam, molten metal or metal salt as heat transfer medium, tubular cracking furnace cracking, fluidized bed cracking, extruder cracking, etc. The existing degradation method has the main defect that the degradation conversion rate is not high.
In order to improve the degradation rate, the chinese patent application CN103242160A discloses a method for preparing methyl methacrylate by composite degradation, comprising the following steps: continuously adding a granular or powdery acrylic material and a catalyst into a screw extruder, advancing the material, firstly melting the material in a melting zone at 240-280 ℃, then cracking the material in a cracking zone at 300-400 ℃, discharging degraded gas through an outlet, and then collecting methyl methacrylate from the degraded gas; the catalyst consists of the following components in parts by weight: 1 part of powder and 1-1.5 parts of peroxide, wherein the powder comprises the following components in parts by weight: 100 parts of oxide, 40-85 parts of chloride and 10-20 parts of organic acid.
Through deep research and experiments, the methyl methacrylate prepared by the method has low yield, high acidity, large residue amount and no practical application value.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method and a device for preparing methyl methacrylate by continuously regenerating waste acrylic, which improve the degradation conversion rate, and simultaneously improve the production efficiency and the safety performance by adopting an enclosed, continuous and automatic operation mode.
In order to solve the above technical problems, the object of the present invention is achieved by the following technical solutions:
the method for preparing methyl methacrylate by continuously regenerating waste acrylic comprises the following steps:
(1) Crushing: crushing waste acrylic to obtain acrylic particles for later use;
(2) And (3) degradation: sequentially degrading acrylic particles obtained in the step (1) through a melting zone, a first-order degradation zone and a second-order degradation zone of a degradation unit to generate methyl methacrylate gas, wherein the melting zone, the first-order degradation zone and the second-order degradation zone are controlled by adopting multiple sections of temperatures, the temperature of the melting zone is controlled at 200-270 ℃ and is increased section by section, the temperature of the first-order degradation zone is controlled at 280-400 ℃ and is increased section by section, and the temperature of the second-order degradation zone is controlled at 380-150 ℃ and is decreased section by section;
(3) And (3) rectification: and (3) rectifying and purifying the methyl methacrylate gas obtained in the step (2) to obtain a methyl methacrylate finished product.
In the method for preparing methyl methacrylate by continuously regenerating waste acrylic acid, the melting zone in the step (2) adopts 4-6 sections of temperature control, preferably 5 sections of temperature control; the first-stage degradation zone adopts 6-8 stages of temperature control, preferably 7 stages of temperature control; the second-order degradation zone adopts 7-9 sections of temperature control, preferably 8 sections of temperature control. The temperature of each section can adopt equal difference arrangement, and different temperature difference values can also be used.
In the method for preparing methyl methacrylate by continuously regenerating waste acrylic, the acrylic particles in the step (2) pass through the degradation unit for 5-20min.
In the method for preparing methyl methacrylate by continuously regenerating waste acrylic, the flow rate of acrylic particles passing through the degradation unit in the step (2) is 3-5kg/min.
In the method for preparing methyl methacrylate by continuously regenerating waste acrylic acid, the rectification in the step (3) adopts multi-stage continuous rectification, including light component removal rectification, primary rectification and secondary rectification, wherein the light component removal rectification, the primary rectification and the secondary rectification adopt different rectification temperatures.
In the method for preparing methyl methacrylate by continuously regenerating waste acrylic acid, the tower top temperature of the light component removal rectification is controlled at 40-60 ℃, and light component substances are separated; the temperature of the top of the first-stage rectification is controlled to be 70-90 ℃, and water is separated out; the tower top temperature of the secondary rectification is controlled at 100-110 ℃, and a methyl methacrylate finished product is separated.
In the method for preparing methyl methacrylate by continuously regenerating waste acrylic acid, polymerization inhibitors are added during light component removal rectification, primary rectification and secondary rectification to prevent polymerization, and the polymerization inhibitors adopt general polymerization inhibitors in the field.
The invention also provides a device for preparing methyl methacrylate by continuously regenerating waste acrylic acid, which comprises a crusher, a degradation unit and a rectifying tower which are sequentially connected, wherein the degradation unit comprises a screw extruder I, a screw extruder II and a screw extruder III which are connected in series, a melting zone, a first-order degradation zone and a second-order degradation zone are respectively formed in the screw extruder I, the screw extruder II and the screw extruder III, and the rectifying tower comprises a light component removal rectifying tower, a first-order rectifying tower and a second-order rectifying tower which are sequentially arranged.
In the device for preparing methyl methacrylate by continuously regenerating waste acrylic, the first screw extruder is a single screw extruder, and the second screw extruder and the third screw extruder are double screw extruders.
In the device for preparing methyl methacrylate by continuously regenerating waste acrylic, the shells of the first screw extruder, the second screw extruder and the third screw extruder are all provided with cast iron heating modules which are arranged in sequence, the cast iron heating modules are controlled by respective independent electric cabinets, and the number of the cast iron heating modules is the same as that of the heating sections.
In the device for preparing methyl methacrylate by continuously regenerating waste acrylic, the cast iron heating module is arranged around the shell of the screw extruder.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention improves the degradation process for preparing methyl methacrylate by continuously regenerating waste acrylic. Three screw extruders connected in series are used for continuously degrading waste acrylic, and meanwhile, the three screw extruders are respectively provided with different temperature control intervals, and multi-section gradient temperature control is adopted, so that the degradation conversion rate is improved to be more than 99%, and the content of a methyl methacrylate crude product is more than 95%.
2. The invention improves the purification process for preparing methyl methacrylate by continuously regenerating waste acrylic. The high-purity methyl methacrylate finished product is obtained by continuous rectification at different temperatures by three groups of rectifying towers, the yield of the finished product can reach more than 90 percent, and the purity can reach more than 99.5 percent.
3. The invention adopts the operation modes of sealing, continuity and automation, thereby improving the production efficiency and the safety performance.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2 is a schematic view of the heating module of the present invention;
reference numerals: 1. a crusher; 2. a screw extruder I; 3. a screw extruder II; 4. a screw extruder III; 5. a light component removal rectifying tower; 6. a primary rectifying tower; 7. a secondary rectification column; 8. cast iron heating module.
Detailed Description
The invention is further described in the following with specific embodiments in conjunction with the accompanying drawings, see fig. 1-2:
device of old and useless ya keli continuous regeneration preparation methyl methacrylate, including breaker 1, degradation unit and the rectifying column that connects gradually, the degradation unit is including screw extruder one 2, screw extruder two 3 and the screw extruder three 4 of establishing ties, forms melting zone, first order degradation district and second order degradation district in screw extruder one 2, screw extruder two 3 and the screw extruder three 4 respectively, the rectifying column is including lightness-removing rectifying column 5, one-level rectifying column 6 and the second grade rectifying column 7 that sets gradually.
Preferably, the first screw extruder 2 is a single screw extruder, and the second screw extruder 3 and the third screw extruder 4 are twin screw extruders.
Referring to fig. 2, the heating module on the screw extruder is set in the following manner: the machine shells of the first screw extruder 2, the second screw extruder 3 and the third screw extruder 4 are respectively provided with cast iron heating modules 8 which are sequentially arranged, the cast iron heating modules 8 are controlled by respective independent electric cabinets, and the number of the cast iron heating modules 8 is the same as that of the heating sections.
Preferably, the cast iron heating module 8 is arranged around the housing of the screw extruder.
The device adopts a closed, continuous and automatic connection mode, and the specific connection structure is as follows: the discharge port of the crusher 1 is connected with the feeding device on the screw extruder I2, the discharge port of the screw extruder I2 is connected with the feed port of the screw extruder II 3, the discharge port of the screw extruder II 3 is connected with the feed port of the screw extruder III 4, the discharge port of the screw extruder III 4 is connected with the middle feed pipeline of the light component removal rectifying tower 5 through a material conveying pipeline, the upper end discharge pipeline of the light component removal rectifying tower 5 is provided with a condenser and a light component collecting storage tank, the lower end discharge pipeline of the light component removal rectifying tower 5 is connected with the middle feed pipeline of the primary rectifying tower 6, the upper end discharge pipeline of the primary rectifying tower 6 is provided with a condenser and a water component collecting storage tank, the lower end discharge pipeline of the primary rectifying tower 6 is connected with the middle feed pipeline of the secondary rectifying tower 7, the upper end discharge pipeline of the secondary rectifying tower 7 is provided with a condenser and a methyl methacrylate collecting storage tank, and the lower end discharge pipeline is provided with a heavy component collecting device.
The method for preparing the methyl methacrylate by continuously regenerating the waste acrylic through the device comprises the following steps:
(1) Crushing: waste acrylic is added into the crusher 1, and the power device drives the crushing devices such as an auger and a cutter in the crusher 1 to crush the acrylic into acrylic particles.
(2) And (3) degradation: sequentially degrading the acrylic particles obtained in the step (1) through a melting zone, a first-order degradation zone and a second-order degradation zone of a degradation unit to generate methyl methacrylate gas, wherein the methyl methacrylate gas comprises the following components:
a. melting: acrylic particles are conveyed into a feeding device on a screw extruder I2 from a discharge port of a crusher 1, the feeding device feeds the acrylic particles into an inner cavity of the screw extruder I2 according to the amount of 3-5kg/min, the inner cavity of the screw extruder I2 forms a melting zone through sectional heating, the heating temperature is controlled to be 200-270 ℃, the heating zone is increased by 5 sections, and the screw of the screw extruder I2 pushes the materials to pass through the temperature zones in sequence and then the materials are output from the discharge port;
b. first-stage degradation: guiding the material output from the discharge port of the screw extruder I2 to enter an inner cavity from a feed port of the screw extruder II 3, heating the inner cavity of the screw extruder II 3 in a segmented manner to form a primary degradation zone, controlling the heating temperature to be 280-400 ℃, increasing the temperature in 7 segments and increasing the temperature in segments, and pushing the material by a screw of the screw extruder II 3 to pass through each temperature zone in sequence and then outputting the material from the discharge port;
c. secondary degradation: guiding the material output from the discharge port of the screw extruder II 3 to enter the inner cavity from the feed port of the screw extruder III 4, heating the inner cavity of the screw extruder II 4 in sections to form a secondary degradation zone, controlling the heating temperature to be 380-150 ℃ and reducing the temperature in sections by 8, and pushing the material by the screw of the screw extruder III 4 to pass through each temperature zone in sequence and then outputting the material from the discharge port;
the time for the acrylic particles to pass through the degradation unit in sequence is controlled to be 5-20min.
(3) And (3) rectification: and (3) sequentially carrying out light component removal rectification, primary rectification and secondary rectification on the methyl methacrylate gas obtained in the step (2), and purifying to obtain a methyl methacrylate finished product, wherein the methyl methacrylate finished product comprises the following components:
a. light component removal and rectification: introducing the methyl methacrylate gas generated in the step (2) into a light component removal rectifying tower 5, controlling the temperature of the top of the light component removal rectifying tower 5 to be 40-60 ℃, discharging the rectified light component substances out of the tower from the top of the tower, condensing the light component substances by a condenser, collecting the light component substances into a light component storage tank, and discharging other methyl methacrylate-containing substances out of the tower from the bottom of the tower;
b. primary rectification: introducing other substances subjected to light component removal and rectification into a primary rectifying tower 6, controlling the temperature of the top of the primary rectifying tower 6 to be 70-90 ℃, discharging components such as rectified water from the top of the tower, condensing the components by a condenser, collecting the components into a water component storage tank, and discharging other substances containing methyl methacrylate from the bottom of the tower;
c. secondary rectification: introducing other substances after the primary rectification into a secondary rectification tower 7, controlling the temperature of the top of the primary rectification tower 7 to be 100-110 ℃, discharging the rectified methyl methacrylate out of the tower from the top of the tower, condensing the methyl methacrylate in a condenser, collecting the methyl methacrylate in a methyl methacrylate storage tank, and discharging other heavy component substances out of the tower from the bottom of the tower.
The yield of the methyl methacrylate finished product obtained by the method reaches over 90 percent, and the purity reaches over 99.5 percent through detection.
The detection method used was gas chromatography, the chromatographic conditions were as follows:
a gas chromatograph: FID detector
A chromatographic column: fused silica capillary column, 30m0.32mmx 0.25 μm
A sample inlet: 250 deg.C
A detector: 300 deg.C
Column temperature: temperature programming is carried out, the initial temperature is 40 ℃, the temperature is kept for 2.5min, the temperature is raised to 73 ℃ at the temperature raising rate of 3 ℃/min, and then the temperature is raised to 250 ℃ at the temperature raising rate of 30 ℃/min.
Sample injection amount: 1 μ L
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, so: equivalent changes made according to the structure, shape and principle of the invention shall be covered by the protection scope of the invention.
Claims (5)
1. The method for preparing methyl methacrylate by continuously regenerating waste acrylic is characterized by comprising the following steps:
(1) Crushing: crushing waste acrylic to obtain acrylic particles for later use;
(2) And (3) degradation: sequentially degrading acrylic granules obtained in the step (1) through a melting zone, a first-order degradation zone and a second-order degradation zone of a degradation unit to generate methyl methacrylate gas, wherein the melting zone, the first-order degradation zone and the second-order degradation zone are controlled by adopting multi-section temperature, the temperature of the melting zone is controlled to be 200-270 ℃ and is increased section by section, the temperature of the first-order degradation zone is controlled to be 280-400 ℃ and is increased section by section, and the temperature of the second-order degradation zone is controlled to be 380-150 ℃ and is decreased section by section;
(3) And (3) rectification: rectifying and purifying the methyl methacrylate gas obtained in the step (2) to obtain a methyl methacrylate finished product;
the melting zone in the step (2) adopts 4-6 sections of temperature control; the first-stage degradation zone adopts 6-8 stages of temperature control; the second-order degradation zone adopts 7-9 sections of temperature control.
2. The method for preparing methyl methacrylate by continuously regenerating waste acrylic acid as claimed in claim 1, wherein the time for allowing acrylic acid particles to pass through the degradation unit in sequence in the step (2) is 5-20min.
3. The method for preparing methyl methacrylate by continuously regenerating waste acrylic acid according to claim 1, wherein the flow rate of acrylic acid particles which sequentially pass through the degradation unit in the step (2) is 3-5kg/min.
4. The method for preparing methyl methacrylate by continuously regenerating waste acrylic acid as claimed in claim 1, wherein the rectification in the step (3) adopts multistage continuous rectification, including light component removal rectification, primary rectification and secondary rectification, and the light component removal rectification, the primary rectification and the secondary rectification adopt different rectification temperatures.
5. The method for preparing methyl methacrylate by continuously regenerating the waste acrylic acid as claimed in claim 4, wherein the tower top temperature of the light component removal rectification is controlled at 40-60 ℃; the tower top temperature of the primary rectification is controlled to be 70-90 ℃; the tower top temperature of the second-stage rectification is controlled to be 100-110 ℃.
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| CN113200854A (en) * | 2021-05-08 | 2021-08-03 | 中石油吉林化工工程有限公司 | Cracking recovery process for producing polymethyl methacrylate |
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| CN109134252A (en) * | 2018-08-23 | 2019-01-04 | 瑞昌荣联环保科技有限公司 | A kind of acrylic cracking recovery system and method using own resource heating |
| CN109761814A (en) * | 2018-12-19 | 2019-05-17 | 霍振辉 | A kind of method that continuous cracking acrylic prepares MMA monomer |
| CN111662175A (en) * | 2020-06-04 | 2020-09-15 | 麻城市中优顺建材科技有限公司 | Method and system for preparing MMA (methyl methacrylate) monomer by recycling waste acrylic |
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2020
- 2020-10-27 CN CN202011165312.XA patent/CN112266324B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3494958A (en) * | 1966-02-05 | 1970-02-10 | Degussa | Production of monomeric cleavage products by thermal decomposition of polymers |
| US5216149A (en) * | 1991-06-07 | 1993-06-01 | Midwest Research Institute | Controlled catalytic and thermal sequential pyrolysis and hydrolysis of mixed polymer waste streams to sequentially recover monomers or other high value products |
| US6469203B1 (en) * | 1998-09-21 | 2002-10-22 | Metallgesellschaft Aktiengesellschaft | Method for depolymerizing polymethylmethacrylate |
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