CN205420240U - Mechanical device of production dichloro nicotinic acid - Google Patents
Mechanical device of production dichloro nicotinic acid Download PDFInfo
- Publication number
- CN205420240U CN205420240U CN201620154690.0U CN201620154690U CN205420240U CN 205420240 U CN205420240 U CN 205420240U CN 201620154690 U CN201620154690 U CN 201620154690U CN 205420240 U CN205420240 U CN 205420240U
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- kettle
- conveyer
- shurry pump
- pipeline
- nicotinic acid
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Abstract
The utility model discloses a mechanical device of production dichloro nicotinic acid, the device belong to medicine and pesticide midbody production field, include: chemical reaction cauldron, filter, chlorination cauldron, centrifuge, hydrolysis reactor, refined cauldron, drying -machine, rubbing crusher, be equipped with first shurry pump and pipeline between chemical reaction cauldron and filter, be equipped with first conveyer between filter and chlorination cauldron, be equipped with second shurry pump and pipeline between chlorination cauldron and centrifuge, be equipped with the second conveyer between centrifuge and hydrolysis reactor, be equipped with third shurry pump and pipeline between hydrolysis reactor and refined cauldron, be equipped with fourth shurry pump and pipeline between refined cauldron and centrifuge, be equipped with the third conveyer between centrifuge and drying -machine, be equipped with the fourth conveyer between drying -machine and rubbing crusher, the last product outlet that is equipped with of rubbing crusher.
Description
Technical field
This utility model belongs to medicine and pesticide intermediate production field, particularly relates to a kind of machinery producing dichloro-nicotinic acid.
Background technology
Dichloro-nicotinic acid, molecular formula C6H4CLNO2, molecular weight 157.55, outward appearance is the clean powder of white, insoluble in cold water, is slightly dissolved in hot water.Dichloro-nicotinic acid is important medicine and pesticide intermediate, can synthesize multiple medical antibacterial element, the medicine for the treatment of cardiovascular disease and disinfectant use in agriculture, insecticide and herbicide etc..The conventional method of the preparation of dichloro-nicotinic acid has following two, one is with 3-picoline as raw material, first generate N-oxygen-3-picoline with hydroperoxidation, then in the presence of acid binding agent diisopropylamine, dropping phosphorus oxychloride is that chlorinating agent carries out ring chlorination in a solvent, obtain chloro--methylpyridine and the mixture of 2-chloro-3-picoline, use the isolation technics that crystallization and rectification method combine, chloro--methylpyridine and 2-chloro-3-picoline can be respectively obtained, 2-chloro-3-picoline carries out pendant chlorine and obtains 2-chloro-3-trichloromethyl pyridine, hydrolysis can obtain dichloro-nicotinic acid further；Two is to be passed through chlorine in phosphorus oxychloride and phosphorus trichloride mixture liquid, temperature controls at about 60 DEG C, until there being remaining chlorine to escape, cool down and be dividedly in some parts nicotinic acid N-oxide, heating mixed liquor reacts 1-1.5 hour in 100～105 DEG C, is stirred for reacting 0.5 hour after question response mixed liquor is transparent, and removed under reduced pressure phosphorus oxychloride, gained residue is cooled to room temperature, and add water to obtain finished product.But this device is to produce with the independently developed production technology of company, and device therefor is company's self assemble.
Summary of the invention
The problem that this utility model mainly solves is to provide a kind of machinery producing dichloro-nicotinic acid, and this device produces dichloro-nicotinic acid with chemical reaction kettle, filter, chlorination tank, centrifugal separator, hydrolysis kettle, refining kettle, dehydrator, pulverizer for equipment.
The technical solution adopted in the utility model is:
A kind of machinery producing dichloro-nicotinic acid, including: chemical reaction kettle 1, filter 2, chlorination tank 3, centrifugal separator 4, hydrolysis kettle 5, refining kettle 6, dehydrator 7, pulverizer 8；nullChemical reaction kettle 1 is provided with the first material inlet 9，The first shurry pump and pipeline 10 it is provided with between chemical reaction kettle 1 and filter 2，Filter 2 is provided with the first waste liquid outlet 11，The first conveyer 12 it is provided with between filter 2 and chlorination tank 3，Chlorination tank 3 is provided with the second material inlet 13，The second shurry pump and pipeline 14 it is provided with between chlorination tank 3 and centrifugal separator 4，Centrifugal separator 4 is provided with the second waste liquid outlet 15，Second conveyor 16 it is provided with between centrifugal separator 4 and hydrolysis kettle 5，Hydrolysis kettle 5 is provided with the 3rd material inlet 17，The 3rd shurry pump and pipeline 18 it is provided with between hydrolysis kettle 5 and refining kettle 6，Refining kettle 6 is provided with the 4th material inlet 19，The 4th shurry pump and pipeline 20 it is provided with between refining kettle 6 and centrifugal separator 4，The 3rd conveyer 21 it is provided with between centrifugal separator 4 and dehydrator 7，The 4th conveyer 22 it is provided with between dehydrator 7 and pulverizer 8，Pulverizer 8 is provided with product outlet 23.
Further technical scheme of the present utility model is:
Described the first conveyer, second conveyor, the 3rd conveyer, the 4th conveyer are drag conveyor.
Described the first shurry pump, the second shurry pump, the 3rd shurry pump, the 4th shurry pump are that resistant material is made, and corresponding pipeline is polyethylene material.
Described chemical reaction kettle, chlorination tank, hydrolysis kettle, refining kettle are 5 tonnes, ceramic liner.
The beneficial effects of the utility model are: provide a kind of machinery producing dichloro-nicotinic acid, and this apparatus structure is simple, it is quick, easy and simple to handle to produce, energy consumption is low；Product purpose is extensive, is important medicine and pesticide intermediate, can synthesize multiple medical antibacterial element, the medicine for the treatment of cardiovascular disease and disinfectant use in agriculture, insecticide and herbicide etc..
Accompanying drawing explanation
Fig. 1 is structure of the present utility model and process flow diagram.
Detailed description of the invention
Embodiment:
Below in conjunction with the accompanying drawings further illustrate use this machinery produce dichloro-nicotinic acid most preferred embodiment particular content:
null1. by the water of formula ratio、Hydrogen peroxide、Sulphuric acid adds chemical reaction kettle 1 by the first material inlet 9 being arranged on chemical reaction kettle 1，When temperature in tune chemical reaction kettle 1 is 40-50 DEG C，Pyridine and the auxiliary agent of formula ratio is added by the first material inlet 9，Dripped the hydrogen peroxide of formula ratio by the first material inlet 9 after now the temperature in chemical reaction kettle 1 being increased to 75 DEG C，Time for adding is 24 hours，After dropping，Controlling temperature is after 78 ± 1 DEG C of reactions 5 hours when being cooled to 35-40 DEG C，Add stirring when sodium carbonate adjusts that the pH value of liquid is 4.5 in still by the first material inlet 9 and stop stirring after half an hour，It is cooled to room temperature，By the first shurry pump being arranged between chemical reaction kettle 1 and filter 2 and pipeline 10, all materials in chemical reaction kettle 1 are sent into filter 2 filter，Liquid portion is discharged by the first waste liquid outlet 11 being arranged on filter 2，Solid portion sends into chlorination tank 3 by the first conveyer 12 being arranged between filter 2 and chlorination tank 3.
null2. the second material inlet 13 by being arranged on chlorination tank 3 adds oxygen phosphorus and the oxide of formula ratio in chlorination tank 3，Stirring is cooled to less than 10 DEG C，Then kettle cover is closed，The triethylamine of formula ratio is dripped by the second material inlet 13 being arranged on chlorination tank 3，Time for adding is 8-10 hour，After dropping，Control insulation 1 hour when temperature is 15 DEG C，Control insulation 1 hour when temperature is 35 DEG C，Controlling temperature is 55 DEG C of insulations 1 hour，Control insulation when temperature is 95 DEG C and terminate reaction after 4 hours，Liquid in still is progressively cooled to 10 DEG C，By the second shurry pump being arranged between chlorination tank 3 and centrifugal separator 4 and pipeline 14, all materials in chlorination tank 3 are sent into centrifugal separator 4 separate，Liquid portion is discharged by the second waste liquid outlet 15 being arranged on centrifugal separator 4，Solid portion sends into hydrolysis kettle 5 by the second conveyor 16 being arranged between centrifugal separator 4 and hydrolysis kettle 5.
3. the 3rd material inlet 17 by being arranged on hydrolysis kettle 5 adds the water of formula ratio, sheet alkali, oxide stirred after 1 hour, heat temperature raising 50-55 DEG C, after being incubated 1 hour, it is continuously heating to 70-75 DEG C, it is incubated 4 hours, then add hydrochloric acid by the 3rd material inlet 17 and adjust pH value 6.5, the activated carbon of formula ratio is added immediately by the 3rd material inlet 17, then all materials in hydrolysis kettle 5 are sent into refining kettle 6 by the 3rd shurry pump and the pipeline 18 being arranged between hydrolysis kettle 5 and refining kettle 6 by insulation decolouring stirring reaction 0.5 hour.
4. the 4th material inlet 19 by being arranged on refining kettle 6 adds the water of formula ratio, when continuing stirring when adjusting pH value to be 7 with alkali liquor while stirring and be progressively warming up to 65-70 DEG C, then insulation is cooled to room temperature half an hour, by the 4th shurry pump being arranged between refining kettle 6 and centrifugal separator 4 and pipeline 20, all materials in refining kettle 6 are sent into centrifugal separator 4 separate, liquid portion is discharged by the second waste liquid outlet 15 being arranged on centrifugal separator 4, solid portion sends into dehydrator 7 by the 3rd conveyer 21 being arranged between centrifugal separator 4 and dehydrator 7 dries, after drying, material is sent into after pulverizer 8 is pulverized by the 4th conveyer 22 being arranged between dehydrator 7 and pulverizer 8 and is obtained finished product, finished product is by products export 23 discharging being arranged on pulverizer 8.
Certainly, this utility model also has other embodiment, and the improvement of any technology, principle and the technique done under without departing from spirit background of the present utility model, within all falling within protection domain of the present utility model.
Claims (4)
1. produce a machinery for dichloro-nicotinic acid, including: chemical reaction kettle (1), filter (2), chlorination tank (3), centrifugal separator (4), hydrolysis kettle (5), refining kettle (6), dehydrator (7), pulverizer (8)；nullIt is characterized in that: chemical reaction kettle (1) is provided with the first material inlet (9)，The first shurry pump and pipeline (10) it is provided with between chemical reaction kettle (1) and filter (2)，Filter (2) is provided with the first waste liquid outlet (11)，The first conveyer (12) it is provided with between filter (2) and chlorination tank (3)，Chlorination tank (3) is provided with the second material inlet (13)，The second shurry pump and pipeline (14) it is provided with between chlorination tank (3) and centrifugal separator (4)，Centrifugal separator (4) is provided with the second waste liquid outlet (15)，Second conveyor (16) it is provided with between centrifugal separator (4) and hydrolysis kettle (5)，Hydrolysis kettle (5) is provided with the 3rd material inlet (17)，The 3rd shurry pump and pipeline (18) it is provided with between hydrolysis kettle (5) and refining kettle (6)，Refining kettle (6) is provided with the 4th material inlet (19)，The 4th shurry pump and pipeline (20) it is provided with between refining kettle (6) and centrifugal separator (4)，The 3rd conveyer (21) it is provided with between centrifugal separator (4) and dehydrator (7)，The 4th conveyer (22) it is provided with between dehydrator (7) and pulverizer (8)，Pulverizer (8) is provided with product outlet (23).
A kind of machinery producing dichloro-nicotinic acid the most according to claim 1, is characterized in that: described the first conveyer, second conveyor, the 3rd conveyer, the 4th conveyer are drag conveyor.
A kind of machinery producing dichloro-nicotinic acid the most according to claim 1, is characterized in that: described the first shurry pump, the second shurry pump, the 3rd shurry pump, the 4th shurry pump are that resistant material is made, and corresponding pipeline is polyethylene material.
A kind of machinery producing dichloro-nicotinic acid the most according to claim 1, is characterized in that: described chemical reaction kettle, chlorination tank, hydrolysis kettle, refining kettle are 5 tonnes, ceramic liner.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620154690.0U CN205420240U (en) | 2016-03-01 | 2016-03-01 | Mechanical device of production dichloro nicotinic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620154690.0U CN205420240U (en) | 2016-03-01 | 2016-03-01 | Mechanical device of production dichloro nicotinic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205420240U true CN205420240U (en) | 2016-08-03 |
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ID=56544557
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620154690.0U Expired - Fee Related CN205420240U (en) | 2016-03-01 | 2016-03-01 | Mechanical device of production dichloro nicotinic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205420240U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU180071U1 (en) * | 2016-05-23 | 2018-05-31 | Федеральное государственное бюджетное учреждение науки "Федеральный исследовательский центр "Казанский научный центр Российской академии наук" | The line for obtaining the drug Na-, Fe-, Ca-polygalacturonate |
-
2016
- 2016-03-01 CN CN201620154690.0U patent/CN205420240U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU180071U1 (en) * | 2016-05-23 | 2018-05-31 | Федеральное государственное бюджетное учреждение науки "Федеральный исследовательский центр "Казанский научный центр Российской академии наук" | The line for obtaining the drug Na-, Fe-, Ca-polygalacturonate |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160803 Termination date: 20190301 |