CN110743486A - Synthesis reactor for oxamide - Google Patents
Synthesis reactor for oxamide Download PDFInfo
- Publication number
- CN110743486A CN110743486A CN201911240313.3A CN201911240313A CN110743486A CN 110743486 A CN110743486 A CN 110743486A CN 201911240313 A CN201911240313 A CN 201911240313A CN 110743486 A CN110743486 A CN 110743486A
- Authority
- CN
- China
- Prior art keywords
- barrel
- synthesis reactor
- inlet
- oxamide
- ammonia gas
- 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.)
- Pending
Links
- YIKSCQDJHCMVMK-UHFFFAOYSA-N Oxamide Chemical compound NC(=O)C(N)=O YIKSCQDJHCMVMK-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 21
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000005192 partition Methods 0.000 claims abstract description 36
- 230000001502 supplementing effect Effects 0.000 claims abstract description 15
- 239000007790 solid phase Substances 0.000 claims abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 230000008676 import Effects 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 20
- 239000000843 powder Substances 0.000 abstract description 9
- 239000000376 reactant Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 description 15
- 239000007795 chemical reaction product Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- LOMVENUNSWAXEN-NUQCWPJISA-N dimethyl oxalate Chemical group CO[14C](=O)[14C](=O)OC LOMVENUNSWAXEN-NUQCWPJISA-N 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
- B01J2219/00763—Baffles
- B01J2219/00765—Baffles attached to the reactor wall
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
- B01J2219/00763—Baffles
- B01J2219/00765—Baffles attached to the reactor wall
- B01J2219/00768—Baffles attached to the reactor wall vertical
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a synthesis reactor for oxamide, which comprises a barrel, and an inlet partition plate and an outlet partition plate which are arranged in the barrel, wherein a feed inlet and a discharge outlet are respectively arranged at two ends of the barrel, a plurality of inlet partition plates and a plurality of outlet partition plates are respectively arranged, the inlet partition plates and the outlet partition plates are sequentially arranged at intervals to form an S-shaped flow channel, the inner wall of the barrel between every two adjacent inlet partition plates or every two adjacent outlet partition plates is connected with an ammonia gas supplementing pipeline and a solid phase discharge port, and the solid phase discharge port is arranged at the bottom of the barrel and is positioned at the downstream of the ammonia gas. The synthesis reactor for oxamide enables the reaction to be complete, continuous, efficient and realizes continuous separation of oxamide powder and reactants.
Description
Technical Field
The invention relates to a synthesis reactor, in particular to a synthesis reactor for oxamide.
Background
Oxamide is a white powder containing nitrogen 31.8%, has no moisture absorption in air, no toxicity and easy storage, has water solubility of 0.016%, and gradually releases ammonia nitrogen and carbon dioxide during hydrolysis or biological decomposition, and is a good urea-aldehyde slow-release fertilizer.
The synthetic route of oxamide is dimethyl oxalate ammonolysis. Mixing the mixed gas of dimethyl oxalate and ammonia gas in a cylinder, and reacting the dimethyl oxalate with the ammonia gas to generate oxamide solid powder and methanol gas. The ammonia gas is more easily separated from the reaction product system, so the reaction system mostly adopts the excess ammonia gas. The prior oxamide gas-phase cylinder mostly adopts a fluidized bed cylinder, because the reaction rate of oxamide and ammonia gas is relatively slow, the residence time of reactants in a reactor is different, and the adoption of the fluidized bed cylinder can cause that part of dimethyl oxalate is not reacted and is discharged out of the cylinder along with reaction products, so that the dimethyl oxalate and the reaction products are difficult to separate, and even the reaction can not be continuously carried out.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an oxamide synthesis reactor which can be used for solving the problems by using an oxamide synthesis cylinder which has adjustable reaction speed, less back mixing and continuous and stable operation.
The invention is realized by the following technical scheme: the utility model provides a synthesis reactor for oxamide, includes the barrel and sets up import baffle and the export baffle in the barrel, the barrel both ends are equipped with feed inlet and discharge gate respectively, import baffle and export baffle all are equipped with a plurality of, and import baffle sets up and forms S type runner with export baffle interval in proper order, forms the reaction unit between adjacent import baffle and the export baffle, and the barrel inner wall connection between two adjacent import baffles or two adjacent export baffles has ammonia to mend pipeline and solid phase discharge port, the solid phase discharge port sets up in the barrel bottom and is located the rear side that the ammonia was mended the pipeline.
In order to facilitate installation, the lower side of the inlet partition plate is connected with the bottom of the inner wall of the cylinder in a welding mode, and the top of the inner wall of the cylinder at the upper side of the outlet partition plate is connected in a welding mode.
In order to facilitate the separation of dimethyl oxalate and reaction products, the heights of the inlet partition plate and the outlet partition plate are both 60-80% of the inner diameter of the cylinder.
In order to adjust the reaction speed and ensure continuous and stable reaction, the side wall of the cylinder between the two inlet clapboards or the two adjacent outlet clapboards is provided with an ammonia gas supplement port, and the ammonia gas supplement pipeline enters from the ammonia gas supplement port and extends into the cylinder.
In order to facilitate uniform reaction, the ammonia gas supplementing pipeline is uniformly provided with a plurality of openings along the axial direction.
In order to facilitate installation, two ends of the cylinder body are respectively provided with a manhole.
The invention has the beneficial effects that: firstly, the barrel is internally divided into a reaction unit and a reaction unit which are connected in series by an inlet clapboard and an outlet clapboard, so that the back mixing is reduced, the residence time of reaction materials, particularly dimethyl oxalate which is difficult to separate from a reaction product system, in the barrel is as consistent as possible, the reaction products are ensured not to contain the dimethyl oxalate, and the continuous separation and continuous reaction in the manufacturing process are ensured; secondly, a reactant inlet pipeline is arranged on the side surface of the cylinder body, and overheated ammonia gas can be introduced into the reactant inlet pipeline, so that the concentration of reactants in a reaction system is increased, the reaction rate of dimethyl oxalate can be improved, and the conversion rate of dimethyl oxalate in the cylinder body is further improved until the dimethyl oxalate is completely reacted; thirdly, an ammonia gas supplementing pipeline is arranged on the side face of the cylinder body, overheated ammonia gas can be introduced into the ammonia gas supplementing pipeline and slightly disturbs reaction products, so that the oxamide powder and the gas phase are mixed more uniformly, the deposition of the oxamide powder in the reaction unit is avoided, and the oxamide powder can be directly discharged from a solid phase discharge port.
Drawings
FIG. 1 is a schematic diagram of the structure of a synthesis reactor for oxamide;
FIG. 2 is a schematic sectional view A-A of a synthesis reactor for oxamide;
FIG. 3 is a schematic cross-sectional view of an inlet baffle and barrel for an oxamide synthesis reactor; (ii) a
FIG. 4 is a schematic sectional view of an outlet baffle and a barrel of a synthesis reactor for oxamide;
in the figure: 1. a barrel; 2. an inlet baffle; 21. an inlet flow aperture; 3. an outlet baffle; 31. an outlet flow aperture; 4. a feed inlet; 5. a discharge port; 6. ammonia is supplemented into the pipeline; 7. a solid phase discharge port; 8. opening a hole; 9. a manhole.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention more readily understood by those skilled in the art, and thus will more clearly and distinctly define the scope of the invention. The directional terms used in the present invention, such as "up", "down", "front", "back", "left", "right", "top", "bottom", etc., refer to the directions of the attached drawings. Accordingly, the directional terms used are used for explanation and understanding of the present invention, and are not used for limiting the present invention.
As shown in figures 1 and 2, a synthesis reactor for oxamide comprises a cylinder 1, and an inlet partition plate 2 and an outlet partition plate 3 which are arranged in the cylinder 1, wherein for the convenience of installation, manholes 9 are respectively arranged at two ends of the cylinder 1, a feed inlet 4 and a discharge outlet 5 are respectively arranged at two ends of the cylinder 1, the discharge outlet 5 is arranged at the bottom of the cylinder 1 far away from the feed inlet 4, a plurality of inlet partition plates 2 and outlet partition plates 3 are respectively arranged, the inlet partition plates 2 and the outlet partition plates 3 are sequentially arranged at intervals to form an S-shaped flow channel, in detail, the bottom of the inlet partition plate 2 is welded with the bottom of the inner wall of the cylinder 1 in a seamless manner, the inlet partition plates 2 and the inner wall of the cylinder 1 form an inlet circulation hole 21, the outlet partition plates 3 are welded with the top of the inner wall of the cylinder 1 in a seamless manner, an outlet circulation hole 31 is formed at one side of the inner wall of the outlet partition plates, the inner wall of the barrel body 1 between two adjacent inlet partition boards 2 or two adjacent outlet partition boards 3 is connected with an ammonia supplementing pipeline 6 and a solid phase outlet 7, the solid phase outlet 7 is arranged at the bottom of the barrel body 1 and is positioned at the rear side of the ammonia supplementing pipeline 6, so that continuous and stable reaction can be realized, the side wall of the barrel body 1 between the two inlet partition boards 2 or the two adjacent outlet partition boards 3 is provided with an ammonia supplementing inlet, the ammonia supplementing pipeline 6 enters from the ammonia supplementing inlet and extends into the barrel body 1, so that uniform reaction can be realized, the ammonia supplementing pipeline 6 is uniformly provided with a plurality of open pores 8 along the axial direction, preferably, the open pores 8 are uniformly provided with 3 open pores 8 along the circumferential direction of the same section of the pipe wall of the ammonia supplementing pipeline 6, and the interval between each open pore.
As shown in fig. 3 and 4, the height of the inlet partition plate 2 and the height of the outlet partition plate 3 are both 60-80% of the inner diameter of the cylinder 1, the lower side of the inlet partition plate 2 is welded with the bottom of the inner wall of the cylinder 1, and the top of the inner wall of the cylinder 1 on the upper side of the outlet partition plate 3 is welded.
The working principle is as follows: at high temperature, dimethyl oxalate gas is introduced from a feed inlet 4 of the cylinder 1, overheated ammonia gas is introduced from an ammonia gas supply pipeline 6, and the ammonia gas uniformly flows out from an opening 8 of the ammonia gas, so that the dimethyl oxalate gas and the ammonia gas fully, completely and continuously react in the reaction unit, oxamide generated by the dimethyl oxalate gas and the ammonia gas is discharged from a solid phase discharge port 7, and the generated reaction gas and unreacted gas are discharged from a discharge port 5 of the cylinder 1.
Compared with the prior art, the synthesis reactor for oxamide has the advantages that the reaction is sufficient, continuous and efficient, the oxamide powder and dimethyl oxalate are continuously separated, the reaction product is ensured not to contain the dimethyl oxalate, in addition, the oxamide powder can be directly discharged from the solid-phase discharge port 7, and the deposition of the oxamide powder in a reaction unit is avoided.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (6)
1. A synthesis reactor for oxamide, characterised by: including barrel (1) and import baffle (2) and the export baffle (3) of setting in barrel (1), barrel (1) both ends are equipped with feed inlet (4) and discharge gate (5) respectively, import baffle (2) and export baffle (3) all are equipped with a plurality of, and import baffle (2) and export baffle (3) interval in proper order set up and form S type runner, and barrel (1) inner wall between two adjacent import baffles (2) or two adjacent export baffles (3) is connected with ammonia and mends pipeline (6) and solid phase discharge port (7), solid phase discharge port (7) set up in barrel (1) bottom and are located the low reaches of ammonia mended pipeline (6).
2. A synthesis reactor for oxamides according to claim 1 characterised in that: the lower side of the inlet partition plate (2) is connected with the bottom of the inner wall of the barrel body (1) in a welded mode, and the top of the inner wall of the upper side barrel body (1) of the outlet partition plate (3) is connected in a welded mode.
3. A synthesis reactor for oxamides according to claim 1 characterised in that: the height of the inlet partition plate (2) and the height of the outlet partition plate (3) are both 60-80% of the inner diameter of the cylinder body (1).
4. A synthesis reactor for oxamides according to claim 1 characterised in that: and an ammonia gas supplementing port is formed in the side wall of the cylinder body (1) between the two inlet partition plates (2) or the two adjacent outlet partition plates (3), and an ammonia gas supplementing pipeline (6) enters from the ammonia gas supplementing port and extends into the cylinder body (1).
5. A synthesis reactor for oxamides according to claim 1 characterised in that: the ammonia gas supplementing pipeline (6) is evenly provided with a plurality of open pores (8) along the axial direction.
6. A synthesis reactor for oxamides according to claim 1 characterised in that: and two ends of the cylinder body (1) are respectively provided with a manhole (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911240313.3A CN110743486A (en) | 2019-12-06 | 2019-12-06 | Synthesis reactor for oxamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911240313.3A CN110743486A (en) | 2019-12-06 | 2019-12-06 | Synthesis reactor for oxamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110743486A true CN110743486A (en) | 2020-02-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911240313.3A Pending CN110743486A (en) | 2019-12-06 | 2019-12-06 | Synthesis reactor for oxamide |
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| CN (1) | CN110743486A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4066706A (en) * | 1975-04-21 | 1978-01-03 | Halcon International, Inc. | Preparation of ethylbenzene hydroperoxide |
| US20040014320A1 (en) * | 2002-07-17 | 2004-01-22 | Applied Materials, Inc. | Method and apparatus of generating PDMAT precursor |
| CN201720057U (en) * | 2010-04-22 | 2011-01-26 | 青岛伊科思技术工程有限公司 | Cyclopentadiene dimerization reaction device |
| CN204891831U (en) * | 2015-08-20 | 2015-12-23 | 北方民族大学 | Gaseous device of horizontal four stirring ammonia oxidation nitrogen dioxide |
| CN106458607A (en) * | 2014-05-13 | 2017-02-22 | 株式会社Lg化学 | Device for manufacturing polysilicon using horizontal reactor and method for manufacturing same |
| CN108745264A (en) * | 2018-07-12 | 2018-11-06 | 常州市金坛区维格生物科技有限公司 | A kind of tubular type continuous esterification device |
| CN109569470A (en) * | 2017-09-28 | 2019-04-05 | 湖北智权专利技术应用开发有限公司 | A kind of aeration reaction kettle |
| CN209490803U (en) * | 2019-01-22 | 2019-10-15 | 常州瑞华化工工程技术股份有限公司 | A kind of horizontal efficient plug flow bubbling reactor |
| CN211190214U (en) * | 2019-12-06 | 2020-08-07 | 东华工程科技股份有限公司 | Synthesis reactor for oxamide |
-
2019
- 2019-12-06 CN CN201911240313.3A patent/CN110743486A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4066706A (en) * | 1975-04-21 | 1978-01-03 | Halcon International, Inc. | Preparation of ethylbenzene hydroperoxide |
| US20040014320A1 (en) * | 2002-07-17 | 2004-01-22 | Applied Materials, Inc. | Method and apparatus of generating PDMAT precursor |
| CN201720057U (en) * | 2010-04-22 | 2011-01-26 | 青岛伊科思技术工程有限公司 | Cyclopentadiene dimerization reaction device |
| CN106458607A (en) * | 2014-05-13 | 2017-02-22 | 株式会社Lg化学 | Device for manufacturing polysilicon using horizontal reactor and method for manufacturing same |
| CN204891831U (en) * | 2015-08-20 | 2015-12-23 | 北方民族大学 | Gaseous device of horizontal four stirring ammonia oxidation nitrogen dioxide |
| CN109569470A (en) * | 2017-09-28 | 2019-04-05 | 湖北智权专利技术应用开发有限公司 | A kind of aeration reaction kettle |
| CN108745264A (en) * | 2018-07-12 | 2018-11-06 | 常州市金坛区维格生物科技有限公司 | A kind of tubular type continuous esterification device |
| CN209490803U (en) * | 2019-01-22 | 2019-10-15 | 常州瑞华化工工程技术股份有限公司 | A kind of horizontal efficient plug flow bubbling reactor |
| CN211190214U (en) * | 2019-12-06 | 2020-08-07 | 东华工程科技股份有限公司 | Synthesis reactor for oxamide |
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