CN101531619B - Device for preparing isocyanate by pyrolyzing aminoalkyl esters - Google Patents
Device for preparing isocyanate by pyrolyzing aminoalkyl esters Download PDFInfo
- Publication number
- CN101531619B CN101531619B CN 200910014822 CN200910014822A CN101531619B CN 101531619 B CN101531619 B CN 101531619B CN 200910014822 CN200910014822 CN 200910014822 CN 200910014822 A CN200910014822 A CN 200910014822A CN 101531619 B CN101531619 B CN 101531619B
- Authority
- CN
- China
- Prior art keywords
- king
- post
- filler
- tower
- oblique
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 125000004103 aminoalkyl group Chemical group 0.000 title claims abstract description 28
- 239000012948 isocyanate Substances 0.000 title claims abstract description 19
- 150000002513 isocyanates Chemical class 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000000047 product Substances 0.000 claims abstract description 27
- 239000006227 byproduct Substances 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 18
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 210000003298 dental enamel Anatomy 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000012856 packing Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 21
- 125000005233 alkylalcohol group Chemical group 0.000 description 19
- 150000002148 esters Chemical class 0.000 description 17
- 230000008569 process Effects 0.000 description 14
- 238000009833 condensation Methods 0.000 description 8
- 230000005494 condensation Effects 0.000 description 8
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- -1 isocyanate compound Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of organic chemical industry production, and relates to a device for preparing isocyanate by pyrolyzing aminoalkyl esters. A major structure comprises a pyrolysis reaction kettle, three tower columns, two H distilling heads and three receiving pots; the top part of the pyrolysis reaction kettle is communicated with the bottom of sieve plate tower columns by a tower body support; the top part of a lower sieve plate tower column is communicated with the bottom of an oblique H distilling head; the top part of the oblique H distilling head is connected with the bottom of a middle packing tower column; an outlet of the oblique H distilling head is respectively communicated with a product receiving pot; the top end of the middle packing tower column is communicated with the bottom end of a horizontal H distilling head; the top part of the horizontal H distilling head is communicated with the bottom of an upper packing tower column; an outlet of the horizontal H distilling head is communicated with a byproduct right receiving pot; and the top part of the packing upper sieve plate tower column and the product receiving pot are communicated with a cold trap respectively. The device has simple structure, reliable principle, easy control of operation and use, high efficiency, strong reaction selectivity and low manufacture cost.
Description
Technical field:
The invention belongs to the apparatus field of organic chemical industry's production technology, relate to a kind of device for preparing isocyanate by pyrolyzing aminoalkyl esters.
Background technology:
Organic isocyanate is the important compound of a class, and the vulcabond of bifunctional has widely application at aspects such as polyurethane industrial, coatings industry, dyestuff and agricultural chemicals.Common industrial production isocyanate compound is that organic amine makes through phosgenation reaction.Although phosgene has higher selectivity, it is the gas that has toxicity, needs closely control, and prepares for a long time and use phosgene, and its leakage is difficult to avoid.Therefore, various countries all actively develop non-phosgene and produce isocyanic ester.At present, the technology and equipment that the non-phosgene process of preparation isocyanic ester relates to is a lot, it is the aminoalkyl esters pyrolysis method that the industrialized technique that is easy to of material impact is wherein arranged, and aminoalkyl esters all produces alkyl alcohol in pyrolytic process, because alkyl alcohol can generate aminoalkyl esters with isocyanate reaction again, so the alkyl alcohol that needs to produce in the reaction process in reaction process in time migrates out system, but because the application prospect with the vulcabond of bifunctional is the widest in the isocyanic ester, and vulcabond has intermediate to produce in pyrolytic process, if the bad meeting of operation control makes the content of vulcabond, yield reduces, reaction preference is poor, even other side reaction such as polymerization occurs, therefore, select good equipment configuration and control the operation of reaction process well to reacting extremely important.
The technology and equipment device of the preparing isocyanate by pyrolyzing aminoalkyl esters of existing patent report is a lot, but research emphasis is not to be placed on conversion unit, is exactly on the catalyzer or successive reaction of reaction; In US Patent No. 4349483, Harder etc. decompose MDC take the silica tube of filling the zinc bits as the reactor pressurization, obtain the MDI of 76.5mol%; And in US Patent No. 4547322, the employing zinc such as Tomonari or aluminium Raschig ring are filler, and MDC is decomposed in pressurization in the vertical reaction tubes of stainless steel, and the yield that obtains MDI is 89.2%wt; These technology all adopt the tubular reactor compressive reaction, and product yield obviously improves but the life-time service pipeline easily stops up, and is not suitable for suitability for industrialized production.In the technique of the preparing isocyanate by pyrolyzing aminoalkyl esters that US Patent No. 6639101, US5449817 and US5326903, US5914428 etc. report, all adopt continuous pyrolysis technique, aminoalkyl ester concentration in the reactive system is very low, generally only have 0.1%～8%, and the concentration of solvent for use and carrier is up to more than 92%, this continuous pyrolysis process equipment manipulation is complicated, dibasic acid esters content is low, monoesters is difficult to recycle, energy consumption is large, the thermal barrier recovery cost is high, do not have economically an advantage, be difficult for realizing commercial scale production.
Summary of the invention:
The object of the invention is to overcome the shortcoming that exists in the prior art, design that a nested structure is simple, long service life, safety coefficient is high, production efficiency is high equipment configuration solve the problems such as normal easy polymerization, the yield that occurs is low in the preparing isocyanate by pyrolyzing aminoalkyl esters technique, the device security coefficient is low.
The aminoalkyl esters pyrolytic process that present device is used is a reversible reaction, and the alkyl alcohol that reaction generates can react with isocyanic ester under pyrolytical condition, regenerates aminoalkyl esters; In addition, isocyanic ester commonly used is vulcabond, vulcabond will experience the process of an intermediate monoisocyanates, make aminoalkyl esters change into vulcabond rather than monoisocyanates fully, its key is to avoid to occur in the pyrolytic process isocyanic ester and the side reactions such as aminoalkyl polyisocyanate polyaddition and isocyanic ester self-polymerization.To achieve these goals, this device is by adopting in different temperature, make aminoalkyl esters under the vacuum tightness, monoisocyanates, product isocyanic ester and alkyl alcohol are at different king-post separating and condensings, namely in the lower sieve plate king-post that links to each other with reactor, make aminoalkyl esters and monoisocyanates realize condensation, return and continue pyrolysis in the pyrolysis still, and product isocyanic ester and alkyl alcohol leave lower sieve plate king-post continuation up, in middle filler king-post, realize separating of product isocyanic ester and alkyl alcohol, product in middle filler king-post after the condensation discharge port by oblique H still head enter in the product receiving tank, alkyl alcohol continues then up that condensation enters in the byproduct receiving tank by flat discharge port to the H still head in upper filler king-post, thereby realizes the recovery of alkyl alcohol; The product that pyrolytic process generates can in time be shifted out from reactor with alkyl alcohol and realize separating at different positions, realizes avoiding when improving plant efficiency because the generation of the polyreaction that isocyanic ester causes.
Agent structure of the present invention comprises the pyrolytic reaction still, three king-posts of upper, middle and lower, oblique, flat receiving tank to two H still heads and three the different purposes in left, center, right, pyrolytic reaction still top links to each other by the tower body bearing with the bottom of sieve plate king-post, the top of lower sieve plate king-post is connected with the bottom of oblique H still head, the top of oblique H still head links to each other with the bottom of middle filler king-post, the discharge port of oblique H still head by the material pipeline respectively with the left receiving tank of product, middle receiving tank is connected, the top of middle filler king-post is connected with flat bottom to the H still head, flat top to the H still head is connected with the bottom of upper filler king-post, flat discharge port to the H still head is connected by the right receiving tank of material pipeline and byproduct, the top of upper filler king-post is connected with cold-trap by vacuum pipeline, and product and byproduct receiving tank are connected with cold-trap by vacuum pipeline respectively.
Because preparing isocyanate by pyrolyzing aminoalkyl esters need to carry out under high temperature, high vacuum, reaction experience intermediate monoisocyanates process, and isocyanate-reactive is higher, under pyrolytical condition easily and alkyl alcohol, aminoalkyl esters react, and product isocyanic ester self also can polymerization reaction take place, thus in whole pyrolytic process alkyl alcohol, monoisocyanates and product isocyanic ester three by realizing timely the separation at different king-posts.Stainless steel with the material contact part in the whole equipment all needs to carry out polished finish, king-post is also different according to different its structures of effect, lower king-post strut is mainly sieve-tray tower, its effect is that monoisocyanates is here separated with product and alkyl alcohol, monoisocyanates condensation backheat solution still continues pyrolysis, middle king-post, upper king-post strut is mainly packing tower, the effect of middle king-post mainly is to realize separating of product and alkyl alcohol, product is condensed and alkyl alcohol is distilled out of, the effect of upper king-post strut mainly is the condensation that realizes alkyl alcohol, thereby realize the recovery of byproduct, conventional condenser can't be realized the condensation of alkyl alcohol under the pyrolysis vacuum condition, the use of the filler king-post of jacketed has realized the recovery of alkyl alcohol.The use of two other H still head is improved rationally the preparing isocyanate by pyrolyzing aminoalkyl esters device more.
The device of preparing isocyanate by pyrolyzing aminoalkyl esters of the present invention, to realize the green synthetic a kind of important technical of isocyanic ester, take the preparing isocyanate by pyrolyzing aminoalkyl esters device as main, be aided with the processing condition of perfect operation and optimization as adopting the control method of temperature programming and program decompression, add high-quality and efficient catalyzer, the non-phosgene production of isocyanic ester is achieved, this technique had both been avoided the use of highly toxic substance phosgene in the traditional technology, various aminoalkyl esters pyrolysis plants have been overcome again in the foreign literature report short work-ing life, product yield is low, reaction preference is poor, the low technological problems that waits of product content makes the non-phosgene suitability for industrialized production become possibility.Preparing isocyanate by pyrolyzing aminoalkyl esters device of the present invention, take time variable control as main, by temperature, pressure and the time of control pyrolytic process, intermediate, product and byproduct that pyrolytic process is produced are realized condensation in different king-posts, reach the purpose of separation, thereby improve the transformation efficiency of aminoalkyl esters and the selectivity of reaction, target product content is higher in the product that obtains, and the recovery of byproduct has realized green synthetic target.
Description of drawings:
Fig. 1 is structural principle schematic diagram of the present invention, comprises pyrolytic reaction still 1, lower sieve plate king-post 2, oblique H still head 3, middle filler king-post 4, flat to H still head 5, upper filler king-post 6 and left, center, right receiving tank 7,8,9.
Embodiment:
Be described further below in conjunction with accompanying drawing and by embodiment.
Embodiment:
The agent structure of the present embodiment comprises pyrolytic reaction still 1, three king-posts 6 of upper, middle and lower, 4 and 2, oblique, flat to two H still heads 3 and 5, three receiving tanks 7 in left, center, right, 8 and 9; The top of pyrolytic reaction still 1 is connected by the tower body bearing with the bottom of lower sieve plate king-post 2, the top of lower sieve plate king-post 2 links to each other with the bottom of oblique H still head 3, the top of oblique H still head 3 links to each other with the bottom of middle filler king-post 4, the discharge port of oblique H still head 3 by the material pipeline respectively with the left receiving tank 7 of product, middle receiving tank 8 is connected, the top of middle filler king-post 4 is connected with flat bottom to H still head 5, flat top to H still head 5 is connected with the bottom of upper filler king-post 6, flat discharge port to H still head 5 is connected by the right receiving tank of material pipeline and byproduct, the top of upper filler king-post 6 is connected with cold-trap A by vacuum pipeline, product and byproduct receiving tank 7,8 and 9 are connected with cold-trap A by vacuum pipeline respectively.
The structure of the pyrolytic reaction still 1 of the present embodiment adopts the enclosed reactor, and volume is 0.5m3, stirs and adopts double mechanical seal, and material adopts SUS316L, and inwall is connected with each king-post and other assemblies by flange through polished finish.
The king-post 2 of the present embodiment is the king-post of jacketed, 3～10 blocks of column plates are arranged in the lower sieve plate king-post 2, and tower body inwall and column plate are the SUS316L material, and all pass through polished finish, logical 140～180 ℃ of thermal oils in the chuck, the sieve diameter of sieve plate king-post is ￠ 10～20mm; Formed by 2 tower joints, the long 450mm of each tower joint, each Ta Jienei has three blocks of column plates, and the tower internal diameter is ￠ 230mm; Connection between two column plates of Ta Jienei adopts threaded stud to connect, and to guarantee the fixing of column plate position, another piece column plate is fixed on the flange connections of two tower joints: 64 holes are arranged on each column plate, and the hole internal diameter is that ￠ 20mm is evenly distributed in the sieve aperture district of column plate.
The oblique still head 3 of the present embodiment is a still head of the H type of jacketed, simple in structure, sloping portion and horizontal plane keep 10～30 ° the elevation angle, to satisfy the control condition from total reflux to full extraction in the pyrolytic process, the logical thermal oil the same with sieve plate king-post 2 temperature in the chuck of H still head 3, its discharge port directly connects valve (can fill automatic control or manually control), unlatching by valve or close to control the amount of extraction or backflow, valve export links to each other with each product receiving tank, and the constant voltage mouth links to each other with the product receiving tank by the material pipeline after directly connecting valve again; Adopt the SUS316L material, internal diameter is ￠ 230mm, and inwall is through polished finish, and the H still head is connected with king-post and each assembly by flange.
The middle filler king-post 4 of the present embodiment is the filler king-post of jacketed, and logical temperature is 40～90 ℃ hot water or deep fat in the chuck, and the filler material in the tower body is glass, pottery or stainless steel; King-post 4 can be comprised of stainless steel or enamel tower joint; King-post consists of with the tower joint of the long 1500mm of a joint, and supporting plate is equipped with in the bottom of tower joint, and filler is placed on the supporting plate in the mode that huddles; Hold-down grid is installed in the top of filler, in case blown by upstream; Filler is ￠ 25mm stainless steel Pall ring filler in the king-post.
The flat structure to H still head 5 of the present embodiment is similar to oblique H still head 3, its sloping portion becomes 5～10 ° the angle of depression with horizontal plane, this angle of depression realizes that H still head 5 does not have the requirement that refluxes in pyrolytic process, when pyrolysis, be equivalent to the effect of a vapour liquid separator, but can realize also that in cleaning equipment total reflux arrives the requirement of full extraction, when the structure of its partial-band chuck satisfies the requirement that nothing refluxes in the production process in addition, also avoid the by product that condensation is got off from the upper filler king-post 6 not to be heated, the constant voltage mouth with link to each other with the byproduct receiving tank by the material pipeline again after valve is connected, pass into hot water or deep fat with filler king-post 4 the same temperature in the chuck; After linking to each other with valve C, flat discharge port to H still head 5 links to each other with byproduct receiving tank 9 by the material pipeline; Adopt the SUS316L material, internal diameter is ￠ 230mm, and inwall is through polished finish; Flat to H still head 5 by flange respectively with king-post 4 with are connected and each assembly is connected.
The filling extract rectification sieve plate king-post 6 of the present embodiment is the filler king-post of jacketed, little than in the filler sieve plate king-post 4 of the filler of filling in the tower, and its material can be stainless steel or enamel; Cat head links to each other with cold-trap by pipeline; King-post is comprised of 2 tower joints, the long 1000mm of each tower joint, and the tower internal diameter is ￠ 230mm, and supporting plate is equipped with in the bottom of tower joint, and filler is placed on the supporting plate in the mode that huddles; Hold-down grid is installed in the top of filler, in case blown by upstream; Filler is ￠ 16mm stainless steel Pall ring filler in the king-post; Logical in the chuck is-10 ℃ refrigerating fulid.
The purpose that the present embodiment is provided with cold-trap A is to cool off incomplete alkyl alcohol and isocyanic ester again cooling here in order to make, thereby reduces it to the infringement of equipment and environment.
Claims (4)
1. the device of a preparing isocyanate by pyrolyzing aminoalkyl esters, it is characterized in that agent structure comprises the pyrolytic reaction still, three king-posts of upper, middle and lower, oblique, flat receiving tank to two H still heads and three the different purposes in left, center, right, pyrolytic reaction still top is connected by the tower body bearing with the bottom of sieve plate king-post, the top of lower sieve plate king-post is connected with the bottom of oblique H still head, the top of oblique H still head links to each other with the bottom of middle filler king-post, the discharge port of oblique H still head by the material pipeline respectively with the left receiving tank of product, middle receiving tank is connected, the top of middle filler king-post is connected with flat bottom to the H still head, flat top to the H still head is connected with the bottom of upper filler king-post, flat discharge port to the H still head is connected by the right receiving tank of material pipeline and byproduct, the top of upper filler king-post is connected with cold-trap by vacuum pipeline, and product and byproduct receiving tank are connected with cold-trap by vacuum pipeline respectively.
2. the device of preparing isocyanate by pyrolyzing aminoalkyl esters according to claim 1 is characterized in that the structure of pyrolytic reaction still adopts the enclosed reactor, and volume is 0.5m
3, stirring and adopt double mechanical seal, inwall is connected with each king-post and assembly by flange through polished finish.
3. the device of preparing isocyanate by pyrolyzing aminoalkyl esters according to claim 1, it is characterized in that king-post is the king-post of jacketed, tower body inwall and column plate lead to 140～180 ℃ of thermal oils all through polished finish in the chuck, the sieve diameter of sieve plate king-post is ￠ 20mm; King-post is comprised of 2 tower joints, the long 450mm of each tower joint, and each Ta Jienei has three blocks of column plates, and the tower internal diameter is ￠ 230mm; Adopt threaded stud to connect between two column plates of Ta Jienei, to guarantee the fixing of column plate position, another piece column plate is fixed on the flange connections of two tower joints: 64 holes are arranged on each column plate, and the hole internal diameter is that ￠ 20mm is evenly distributed in the sieve aperture district of column plate.
4. the device of preparing isocyanate by pyrolyzing aminoalkyl esters according to claim 1, it is characterized in that the filler king-post is the filler king-post of jacketed, logical temperature is 40～90 ℃ hot water or deep fat in the chuck, and the filler material in the tower body is glass, pottery or stainless steel; King-post is comprised of stainless steel or enamel tower joint, and king-post consists of with the tower joint of the long 1500mm of a joint, and supporting plate is equipped with in the bottom of tower joint, and filler is placed on the supporting plate in the mode that huddles; Hold-down grid is installed in the top of filler, in case blown by upstream; Filler is ￠ 25mm stainless steel Pall ring filler in the king-post.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910014822 CN101531619B (en) | 2009-04-21 | 2009-04-21 | Device for preparing isocyanate by pyrolyzing aminoalkyl esters |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910014822 CN101531619B (en) | 2009-04-21 | 2009-04-21 | Device for preparing isocyanate by pyrolyzing aminoalkyl esters |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101531619A CN101531619A (en) | 2009-09-16 |
| CN101531619B true CN101531619B (en) | 2013-04-03 |
Family
ID=41102500
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910014822 Active CN101531619B (en) | 2009-04-21 | 2009-04-21 | Device for preparing isocyanate by pyrolyzing aminoalkyl esters |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101531619B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844064B (en) * | 2010-05-18 | 2014-09-24 | 中国科学院过程工程研究所 | Reactor and method for preparing isocyanate by gas phase pyrolysis |
| CN102260193B (en) * | 2010-05-26 | 2013-11-06 | 中国科学院过程工程研究所 | Method and reaction device for preparing isocyanate through thermal decomposition of carbamate by molecular distillation technology |
| CN102675154B (en) * | 2011-03-11 | 2013-11-06 | 中国科学院过程工程研究所 | Separation and purification device and method for preparing methylene diphenyl diisocyanate (MDI) complex product by utilizing pyrolysis of carbamate |
| CN103990291B (en) * | 2014-04-21 | 2017-02-15 | 开封华瑞化工新材料股份有限公司 | Xylylene diisocyanate rectification apparatus and rectification method thereof |
| CN113024417B (en) * | 2021-05-27 | 2021-08-31 | 中国科学院过程工程研究所 | Method and device for strengthening separation in isocyanate preparation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3870739A (en) * | 1973-03-05 | 1975-03-11 | Air Prod & Chem | Isocyanates from urethanes |
| US5284969A (en) * | 1991-11-14 | 1994-02-08 | Bayer Aktiengesellschaft | Process for the production of polyisocyanates |
| CN1850792A (en) * | 2006-05-23 | 2006-10-25 | 中国科学院山西煤炭化学研究所 | Method for preparing diphenyl methane vulcabond |
-
2009
- 2009-04-21 CN CN 200910014822 patent/CN101531619B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3870739A (en) * | 1973-03-05 | 1975-03-11 | Air Prod & Chem | Isocyanates from urethanes |
| US5284969A (en) * | 1991-11-14 | 1994-02-08 | Bayer Aktiengesellschaft | Process for the production of polyisocyanates |
| CN1850792A (en) * | 2006-05-23 | 2006-10-25 | 中国科学院山西煤炭化学研究所 | Method for preparing diphenyl methane vulcabond |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101531619A (en) | 2009-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101531619B (en) | Device for preparing isocyanate by pyrolyzing aminoalkyl esters | |
| CN100537511C (en) | Method and equipment for continuous esterification production of adipic acid dimethyl ester | |
| CN100532338C (en) | Process for producing benzyl chlorides chemical compound | |
| CN201031140Y (en) | Device for producing ultra-clear and high-purity | |
| CN100497161C (en) | Method and equipment for preparing super clean, high purified hydrofluoric acid | |
| CN102101651A (en) | Method and device for refining chlorine hydride byproduct and recovering trifluoromethane in production of monochlorodifluoromethane | |
| CN110218151A (en) | A kind of device and method that tower reactor Flash Type heat pump reactive distillation prepares propyl propionate | |
| CN104117358A (en) | Compound catalyst and method for synthesizing aliphatic or cyclic diisocyanate in presence of catalyst | |
| CN102267868A (en) | Industrial production apparatus for trichloroethylene | |
| CN113603718A (en) | Vacuum process for cracking dimethyl dichlorosilane hydrolysate | |
| CN201762266U (en) | Trichloroethylene industrialized production device | |
| CN109456207B (en) | Preparation method of 3-aminopropanol | |
| CN201603410U (en) | Energy-saving continuous alcohol-rectification recovery tower | |
| CN108946668B (en) | Preparation process of anhydrous hydrogen fluoride | |
| CN101844064B (en) | Reactor and method for preparing isocyanate by gas phase pyrolysis | |
| CN217120204U (en) | Device for producing tertiary amine through continuous reaction of adiabatic fixed bed | |
| CN103980159A (en) | Reaction system for preparing isocyanate by carrying out continuous pyrolysis on amino alkyl acid ester | |
| CN101538192A (en) | Enyl phenol refining plant and method thereof | |
| CN101481362B (en) | Method for preparing hexamethylene imine | |
| CN220695879U (en) | Improved generation high efficiency large-scale sieve evaporates ammonia tower | |
| CN106588655B (en) | Device and production process for synthesizing dimethyl carbonate by using reaction of urea and methanol | |
| CN213824717U (en) | Liquid descending chlorination tower in tower | |
| CN111689835A (en) | Preparation of C by cracking F222F4System and method for recovering trifluoroethylene in process | |
| CN209302214U (en) | A kind of industrial acenaphthylene fractionating device utilizing waste heat for refrigeration equipment | |
| CN215365548U (en) | Pretreatment device before aniline rectification |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20160114 Granted publication date: 20130403 |
|
| RINS | Preservation of patent right or utility model and its discharge | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20160714 Granted publication date: 20130403 |
|
| RINS | Preservation of patent right or utility model and its discharge | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20170110 Granted publication date: 20130403 |
|
| RINS | Preservation of patent right or utility model and its discharge | ||
| PD01 | Discharge of preservation of patent | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20200710 Granted publication date: 20130403 |
|
| PP01 | Preservation of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20200710 Granted publication date: 20130403 |
|
| PD01 | Discharge of preservation of patent | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20210110 Granted publication date: 20130403 |
|
| PP01 | Preservation of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20210110 Granted publication date: 20130403 |
|
| PD01 | Discharge of preservation of patent | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20240110 Granted publication date: 20130403 |