CN1560021A - Process of preparaing methyl acrylate by waste organic glass and apparatus thereof - Google Patents
Process of preparaing methyl acrylate by waste organic glass and apparatus thereof Download PDFInfo
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- CN1560021A CN1560021A CNA2004100264400A CN200410026440A CN1560021A CN 1560021 A CN1560021 A CN 1560021A CN A2004100264400 A CNA2004100264400 A CN A2004100264400A CN 200410026440 A CN200410026440 A CN 200410026440A CN 1560021 A CN1560021 A CN 1560021A
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Abstract
The invention relates to a technique of preparing methyl methacrylate (MMA) by waste organic glass and its device, disclosing a semicontinuous cracking method and an integrated cracking and distilling device. It implements a technique of combining cracking and distilling and the technical courses: crushing the waste organic glass, adding the made glass particles in cracking kettles continuously, orderly and properly, temperature range 140-380 deg.C, as the glass particles reaches a certain quantity, stopping feeding and making final-period cracking and processing, where the average time of cracking and distilling in each a kettle in a cycle (by 1000 kg raw material) is 5-7 hours. On at 140 deg.C can it generate cracked MMA; the MMA product at 140-280 deg.C is dehydrated and becomes a transparent and clear liquid; the MMA purity is 97-99% and the MMA yield is 85-92%.
Description
Technical field
The present invention relates to the recycling of waste and old organic glass, specifically be meant with the waste and old organic glass to be that raw material adopts semicontinuous cracking technology and cracking and distillation integrated apparatus to prepare methyl methacrylate.
Background technology
Discarded synthetic glass after cutting material that produces in waste material that occurs in the synthetic glass production process and the mechanical workout and chip and the use, as: billboard, light fixture, lamp box, artwork, dalle, mahjong or the like, according to present incomplete statistics, its amount accounts for the 30-40% of synthetic glass output.Along with increasing of synthetic glass application and development and waste and old organic glass, theoretically, waste and old synthetic glass and turnout are suitable.Cracking is particularly carried out in the recycling of waste and old organic glass, produces monomers methyl methacrylate (English: Methyl Methacrylate again; Abbreviation: MMA) on the utilization of resources, environment protection and economic benefit, all be of great importance.
Generally can be divided into interrupter method and continuous processing in the middle of the cracking technology practice of waste and old organic glass.Interrupter method is prevailing a kind of method, also is the method routinely that present many manufacturers generally use.The main processes of this method is at first raw material to be carried out the intermittent type cracking in reactor, obtains thick MMA monomer; Second step was the thick MMA monomer that obtains after the cracking to be put into still kettle carry out intermittent fractionation again, to obtain smart monomer M MA product.Interrupter method exists many shortcomings, mainly is that its non-cutting time of each still production operation is long, and will account for 1/3rd of each still cracking time non-cutting time (time of the cooling after containing reinforced, cracking and finishing, operation such as slag tap).The time of scission reaction reaches 14-18 hour, after cracking is finished, has only question response still cooling, does not have hot gas to go out Shi Caike to slag tap, and the time will be delayed 5-7 hour.Therefore use this method energy expenditure big, efficient is lower, and every batch operation time is long.
Some aspect of continuous cracking method of waste and old organic glass is better than interrupter method, it can overcome some defectives that interrupter method exists, but itself since need satisfy charging continuously, slag tap continuously and requirements such as control stabilization, and make the device more complicated, operation easier is big, is difficult to grasp the production operation condition.Because the waste and old organic glass source is different, form complexity again, the content instability is difficult to grasp the cracking terminal point, and yield is descended.Do not find also at present that domestic production producer has the employing continuous processing to produce.
Summary of the invention
Purpose one of the present invention is long in order to overcome the non-cutting time that batch process exists, and it is frequent to slag tap, and causes each still production cycle to reach individual hour defective of nearly 20-30; The 2nd, be difficult to grasp in order to overcome continuous processing cracking technology equipment complexity, operational requirement height, explained hereafter, cause the defective that is not adopted by manufacturer; Overcome in above-mentioned two kinds of methods cracking simultaneously and separate the shortcoming that energy expenditure is big with distillation.
The inventor has carried out repetitious improvement, test at existing technology in the background technology and equipment thereof, perfect basically utilizes waste and old organic glass to implement technology and the device thereof of the smart monomer M MA of the integrated preparation of semicontinuous cracking and cracking and distillation.Make operating procedure of the present invention simplify, shorten non-cutting time greatly, and production unit is simple in structure, is easy to grasp and operation, and the purity of product and yield are all higher.
The present invention addresses the above problem and achieves the above object and is achieved by the following technical solution: the technology and the device thereof that prepare methyl methacrylate with waste and old organic glass, described technology is to adopt semicontinuous cracking process, and described device is cracking and distillation integrated apparatus.
It is cracking and distillation integrated apparatus that waste and old organic glass of the present invention prepares the described device of methyl methacrylate, this device is that cracking still is provided with distillation tower, tower is built-in with high efficiency packing, cat head is provided with condenser, water cooler and reflux and water trap etc., also is provided with cracking later stage vacuum and extracts the condensation gathering system out on cracking still.
Cracking still described in the present invention has at the bottom of flat ellipse, the circular heating kettle, also can be the heating kettle of dish or ball shape at the bottom of.Can guarantee at the bottom of the heating kettle of these shapes that the heating-surface area and the ratio of cracking material amount reach the big ratio of trying one's best.And existing cracking still is flat cylindrical, and its heating-surface area is about 2m with the ratio of cracking material amount
2/ 1t, and use this cracking still, its heating-surface area approximates 6m with the ratio of cracking material amount
2/ 1t.Therefore big, fast, the rate of cleavage raising of conducting heat of this cracking still heat transfer area.
Cracking still described in the present invention is provided with vacuum and extracts the condensation gathering system out, described vacuum is extracted the condensation gathering system out and is made up of vacuum pump, snubber, storage tank, condenser etc., cracking still connects condenser, and condensator outlet connects storage tank, and storage tank connects snubber to vacuum pump.It is will contain the lower yellow cracked gas condensation of MMA to collect that this vacuum is extracted condensation gathering system one out, without the distillation tower that links with cracking still, in order to avoid pollute water distilling apparatus.The 2nd, under reduced pressure material cracking in the still can be got cleaner, can make still without the cooling directly slag tap.
The semicontinuous cracked technology that waste and old organic glass described in the present invention prepares methyl methacrylate is: with heating pyrolyze and distillation in the adding cracking still continuous, orderly, an amount of after the waste and old organic glass raw material pulverizing, cracking temperature is 140-380 ℃, and the cracking of each still in the one-period (in the 1000kg raw material) is 5-7 hour with distillation combine operations time average.Wherein: the smart monomer M MA of cracked product output is arranged in the time of 140 ℃, and contain small amount of moisture; After the product MMA dehydration that 140-280 ℃ of temperature range implosion solves, be transparent clear liquid; In the time of more than 280 ℃, a small amount of yellow or faint yellow split product output are arranged.
The technological process that waste and old organic glass prepares the semicontinuous cracking process of methyl methacrylate is: (1), elder generation deposit the pellet behind the waste and old organic glass raw material crushing into the material storage storehouse; (2), by in device for transporting objects adding cracking that the waste and old organic glass particle is continuous, orderly, an amount of and the integrated scission reaction still of distillation, until the total stuff amount that adds stops to add when reaching 7-8 times of cracking still volume; Temperature is controlled at 140-280 ℃; Scission reaction in this temperature is collected distillate in the period, is smart monomer M MA after dehydration; (3) stop charging after, when temperature has a spot of yellow or faint yellow split product to separate out in time more than 280 ℃, at this moment by vacuum extract out, the condensation gathering system collects this part split product in the cracking still; (4), slag tap after cracking is finished.
The present invention has realized that cracking and distillation are united and semi continuous operation technology owing to adopt semicontinuous cracking process and cracking and distillation integrated apparatus.Therefore positively effect of the present invention and excellent part are as follows:
1, equipment and processing parameter advanced person, can make waste and old organic glass carry out orderly cracking, its purity and productive rate are higher, the methyl methacrylate product that goes out cracking temperature 140-280 ℃ of scope cracking is a transparent clear liquid, purity is 97-99% (saponification method), and productive rate is 85-92% (product volume/cracking material amount).
2, cracking and distillation integral process and device do not need to add still kettle in addition, have saved the operation of rectifying and have saved energy, make equipment configuration oversimplify, and production cost reduces.
3, eliminate repolymerization phenomenon in still kettle, also got rid of methyl methacrylate dimer, tripolymer and run possibility in the product, saved the distillatory energy, reduced loss, be included in the polymerization in the distillation, the losses such as volatilization in the system.
4, the throughput of cracking and distillation integrated apparatus is big, and a semicontinuous cracking still is equivalent to the cracking still of 3-4 equal volume in the interrupter method.
Testing data shows: the best quality of technology of the present invention and product MMA that device obtained and prior art is suitable, meets relevant application requiring.Concrete data list is as follows:
The domestic high-quality cracking of index synthetic typical products product product of the present invention
(actual measurement of groove sample)
MMA purity/% 99.9 98 98.5
(saponification method)
Colourity≤10≤15 14
(HPHA)
Acidity/% 0.003 0.003 0.003
Water content/% 0.03 0.03 0.03
(in MMA)
Description of drawings
The present invention is further described below in conjunction with drawings and Examples:
Fig. 1 is semicontinuous cracking process cracking of the present invention and the integrated block diagram of distillation;
Fig. 2 is cracking of the present invention and distillation integrated apparatus synoptic diagram.
Shown in the figure: 1, cracking still; 2, distillation tower; 3, thermometer mouth; 4, continuously feeding mouth; 5, vacuum is extracted out and is collected mouth; 6, slag notch.21, condenser; 22, water cooler; 23, water trap; 51, condenser; 52, storage tank; 53, snubber; 54, vacuum pump.
Embodiment
Shown in accompanying drawing 1,2, the present invention is semicontinuous cracking process and cracking and distillation integrated apparatus, and this device is that cracking still 1 is provided with distillation tower 2, and tower is built-in with high efficiency packing, and cat head is provided with condenser 21, water cooler 22, water trap 23; Be flat ellipse, circular at the bottom of the cracking still described in the present invention, or dish, and spheroid.Can guarantee at the bottom of the cracking still of this shape that the heating-surface area and the ratio of cracking material amount reach the big ratio of trying one's best.On cracking still, also be provided with cracking later stage vacuum and extract the condensation gathering system out, described vacuum is extracted the condensation gathering system out and is made up of vacuum pump 54, snubber 53, storage tank 52, condenser 51 etc., connect condenser 51 on the cracking still 1, condensator outlet connects storage tank 52, and storage tank connects snubber 53 to vacuum pump 54; Cracking still 1 is provided with continuously feeding mouth 4, thermometer mouth 3, slag notch 6.Technology of the present invention is continuously to drop into heating pyrolyze and distillation in the reactor 1 by the opening for feed on the cracking still 14 after the waste and old organic glass raw material pulverizing, and temperature is controlled at 140-280 ℃; Scission reaction in this temperature is collected distillate in the period, is smart monomer M MA after dehydration.After stopping charging,, at this moment collect this part split product in the cracking still by vacuum extraction, condensation gathering system when temperature has a spot of yellow or faint yellow split product to separate out in time more than 280 ℃.When not having the splitting gas extraction, stop cracking, implement to slag tap.
Apparatus of the present invention implementation example is as follows: the cracking still that this device designs and produces can be put into waste and old organic glass particle 1000kg; Be high efficiency packing in the distillation tower that connects on the cracking still, the top is provided with condenser, water cooler and reflux and water trap, and cracked gas comes out to collect with liquid state after the condensation cooling from cat head.The kettle cover place is provided with continuous feeding and vacuum collection system.The waste and old organic glass pellet of pulverizing initially adds 700kg in cracking still, behind the feeding water coolant, begins heat temperature raising in the condenser.A small amount of cracked gas output is just arranged in the time of 140 ℃.Cracked gas carries out mass transfer, exchange by the liquid of king-post and condensing reflux, reaches the purpose of rectifying.Collect after the condensation cooling from the gas that cat head comes out.Treat after the cracking to 2 hour, about 200 ℃ of cracking temperatures, the beginning continuously feeding, the speed and the rate of cleavage of its charging are suitable, through 39 hours continuously feeding, add the 7200kg pellet altogether.Stop to feed in raw material, continue material cracking in the still.After 2 hours, it is little when yellow that the liquid material that cracking is come out begins to become, and stops the rectifying discharging, starts the vacuum collection system, begins simultaneously to heat up, and after 80 minutes, do not had splitting gas and extracted out, stops cracking, implements to slag tap.
The smart monomer M MA that collects via cracking and water distilling apparatus after dehydration, product 6270kg, outward appearance is pure white limpid transparent liquid.It is 98.5% that saponification method detects MMA purity content; In the waste and old organic glass particle is benchmark, and productive rate is 87.1%.Extract the yellow material 252kg that system and device is collected out via vacuum, output capacity is 3.5%.This operational cycle comprises cracking and whole non-cutting times, amounts to 45 hours, in the average one-period each still (in the 1000kg raw material) consuming time be 6.3 hours.
Claims (6)
1, waste and old organic glass prepares the device of methyl methacrylate, it is characterized in that described device is cracking and distillation integrated apparatus, this device is that cracking still is provided with distillation tower, tower is built-in with high efficiency packing, cat head is provided with condenser, water cooler and reflux and water trap, also is provided with the later cleavage vacuum and extracts the condensation gathering system out on cracking still.
2, waste and old organic glass according to claim 1 prepares the cracking and distillation integrated apparatus of methyl methacrylate, it is characterized in that at the bottom of the described cracking still be flat ellipse, circular, or dish and spheroid.
3, waste and old organic glass according to claim 1 and 2 prepares the cracking and distillation integrated apparatus of methyl methacrylate, it is characterized in that vacuum extracts the condensation gathering system out and be made up of vacuum pump, snubber, storage tank, condenser, cracking still connects condenser, condensator outlet connects storage tank, and storage tank connects snubber and arrives vacuum pump again.
4, waste and old organic glass prepares the semicontinuous cracking technology of methyl methacrylate, it is characterized in that described technology is: cracking and distillation in the adding cracking heating kettle that the pellet after the waste and old organic glass raw material pulverizing is orderly continuously, when being long-pending 7-8 times of still, add-on stops adding, temperature range is 140-380 ℃, cracking of each still (in the 1000kg raw material) and distillation time average out to 5-7 hour.
5, waste and old organic glass according to claim 4 prepares the semicontinuous cracking technology of methyl methacrylate, it is characterized in that this technological process is:
(1), in adding cracking that the pellet behind the waste and old organic glass raw material crushing is orderly continuously earlier and the integrated scission reaction still of distillation, temperature is controlled at 140-280 ℃; Collect distillate in scission reaction in period, after dehydration, be smart monomer product;
(2) stop charging,, at this moment enable vacuum and extract the condensation collection device out, collect this part split product in the cracking still when temperature then has yellow or faint yellow split product to separate out in time more than 280 ℃;
(3), no splitting gas extracts out, stops the cracking operation, implement to slag tap.
6, waste and old organic glass according to claim 5 prepares the semicontinuous cracking technology of methyl methacrylate, it is characterized in that: cracked methyl methacrylate output is arranged in the time of 140 ℃, and contain small amount of moisture; The methyl methacrylate product that solves 140-280 ℃ of temperature range implosion is a transparent clear liquid; Purity is 97-99%, and productive rate is 85-92%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410026440 CN1235861C (en) | 2004-03-11 | 2004-03-11 | Process of preparaing methyl acrylate by waste organic glass and apparatus thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410026440 CN1235861C (en) | 2004-03-11 | 2004-03-11 | Process of preparaing methyl acrylate by waste organic glass and apparatus thereof |
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| Publication Number | Publication Date |
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| CN1560021A true CN1560021A (en) | 2005-01-05 |
| CN1235861C CN1235861C (en) | 2006-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140183A (en) * | 2010-12-16 | 2011-08-03 | 浙江省天正设计工程有限公司 | Process and technological equipment for continuously cracking and recycling waste organic glass |
| CN103130945A (en) * | 2013-03-27 | 2013-06-05 | 苏州双象光学材料有限公司 | Polymethyl methacrylate (PMMA) continuous production process for long-time operation without accumulation |
| CN103242160A (en) * | 2013-05-23 | 2013-08-14 | 上虞奥莱法压克力材料科技有限公司 | Method for preparing methyl methacrylate by composite degradation |
| CN105056562A (en) * | 2015-08-07 | 2015-11-18 | 无锡市悦丰化工有限公司 | Distillation tower for production of methyl methacrylate |
| CN112266324A (en) * | 2020-10-27 | 2021-01-26 | 张明 | Method and device for preparing methyl methacrylate by continuously regenerating waste acrylic |
| CN113024378A (en) * | 2021-03-15 | 2021-06-25 | 瑞昌荣联环保科技有限公司 | Acrylic recovery method |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130946B (en) * | 2013-03-27 | 2015-07-29 | 苏州双象光学材料有限公司 | The continous way production technique of polymethylmethacrylate |
| CN103130947B (en) * | 2013-03-27 | 2015-07-29 | 苏州双象光学材料有限公司 | Optical-grade polymethylmethacrylacontinuous production technique |
-
2004
- 2004-03-11 CN CN 200410026440 patent/CN1235861C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140183A (en) * | 2010-12-16 | 2011-08-03 | 浙江省天正设计工程有限公司 | Process and technological equipment for continuously cracking and recycling waste organic glass |
| CN102140183B (en) * | 2010-12-16 | 2012-11-28 | 浙江省天正设计工程有限公司 | Process and technological equipment for continuously cracking and recycling waste organic glass |
| CN103130945A (en) * | 2013-03-27 | 2013-06-05 | 苏州双象光学材料有限公司 | Polymethyl methacrylate (PMMA) continuous production process for long-time operation without accumulation |
| CN103130945B (en) * | 2013-03-27 | 2014-12-10 | 苏州双象光学材料有限公司 | Polymethyl methacrylate (PMMA) continuous production process for long-time operation without accumulation |
| CN103242160A (en) * | 2013-05-23 | 2013-08-14 | 上虞奥莱法压克力材料科技有限公司 | Method for preparing methyl methacrylate by composite degradation |
| CN103242160B (en) * | 2013-05-23 | 2014-10-08 | 上虞奥莱法压克力材料科技有限公司 | Method for preparing methyl methacrylate by composite degradation |
| CN105056562A (en) * | 2015-08-07 | 2015-11-18 | 无锡市悦丰化工有限公司 | Distillation tower for production of methyl methacrylate |
| CN112266324A (en) * | 2020-10-27 | 2021-01-26 | 张明 | Method and device for preparing methyl methacrylate by continuously regenerating waste acrylic |
| CN112266324B (en) * | 2020-10-27 | 2023-02-28 | 张明 | Method and device for preparing methyl methacrylate by continuously regenerating waste acrylic |
| CN113024378A (en) * | 2021-03-15 | 2021-06-25 | 瑞昌荣联环保科技有限公司 | Acrylic recovery method |
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| CN1235861C (en) | 2006-01-11 |
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