CN206173250U - Serialization apparatus for producing of stearic acid acyl chlorides - Google Patents
Serialization apparatus for producing of stearic acid acyl chlorides Download PDFInfo
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- CN206173250U CN206173250U CN201621131150.7U CN201621131150U CN206173250U CN 206173250 U CN206173250 U CN 206173250U CN 201621131150 U CN201621131150 U CN 201621131150U CN 206173250 U CN206173250 U CN 206173250U
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- acyl chloride
- chloride reaction
- kettle
- stearic
- acyl chlorides
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Abstract
The utility model belongs to the technical field of organic synthesis, specificly relate to a serialization apparatus for producing of stearic acid acyl chlorides. This kind of serialization apparatus for producing of stearic acid acyl chlorides includes acyl chlorides reaction system, stearic acid acyl chlorides purification system and vent gas treatment system in in proper order, the acyl chlorides reaction system includes acyl chlorides reation kettle, and this acyl chlorides reation kettle's cauldron top department is equipped with the injection reactor, and the liquid phase import and the reactant outlet of this injection reactor are located both ends respectively, and gas -phase inlet is located one side of injection reactor, the delivery pump and reaction circulating pump that respectively with injection reactor link to each other are equipped with in acyl chlorides reation kettle's bottom. This apparatus for producing adopts continuity method, and various operating parameters are stable, and the maximum reaction rate that has accelerated has improved purity, stability and the yield of product, has reduced the production volume of accessory substance.
Description
Technical field
This utility model belongs to the technical field of organic synthesiss, is specifically related to a kind of continuous prodution of stearic
Device.
Background technology
Stearic, also known as octadecanoyl chlorine, with following purposes：As colour cinefilm colour coupler（Such as 535,
577,169,133 etc.）Intermediate；For producing amide anhydride etc.；What the esterification as alcohol and other organic compound synthesized
Raw material；For producing papermaking neutral sizing agent AKD (alkyl ketene dimer).
Stearic（Octadecanoyl chlorine）Through the popularization of nearly more than ten years, its market consumption rises year by year.Prior art
Middle employing batch production, it is specific as follows：The stearic acid of metering is added in enamel reaction still, under stirring condition Jing pipelines press than
Example adds catalyst and activated carbon, is passed through phosgene, takes jacket steam or cooling water mode to keep in kettle temperature of charge in 60-70
DEG C, when accumulative phosgene addition reaches definite value, stop thang-kng, product is analyzed, while acyl chloride reaction kettle is incubated about 1
Hour, product analyses are unqualified, continue thang-kng；Qualified product, then carry out next step N2Light program is caught up with, catches up with the light time to be about
8 ~ 10h, when material free chlorine is less than or equal to 0.5% in kettle, kettle temperature is maintained at 40 DEG C, waits and enters next step filter.
Crude product stearic obtains product stearic Jing after sucking filtration or filter pressing.
Stearic at this stage has been enter into large-scale production period, but the design of main flow device always according to batch process life
Product is simply amplified, and batch process production process has problems with：（1）The quality poor repeatability of product, per batch products
Purity has difference；（2）Life cycle of the product is long, and phosgene utilization rate is low, increased product cost；（3）The operation ginseng of batch process
Several dependencies to operator are stronger, and the error of the occasionality of operator, working condition and operating technology level all can become
The obstacle of product with stable quality.
The content of the invention
The purpose of this utility model is to provide a kind of continuous metaplasia of stearic for above-mentioned defect
Device is produced, the process units adopts continuity method, various operating parameters to stablize, farthest accelerates reaction rate, shortens
Production cycle, the utilization rate of phosgene is improve, reduces improve purity, stability and the yield of product while production cost,
Reduce the yield of by-product.
The technical solution of the utility model is：A kind of continuous production device of stearic, it is anti-including acyl chlorides successively
Answer system, stearic purification system and exhaust treatment system；The acyl chloride reaction system includes acyl chloride reaction kettle, the acyl chlorides
Injection reactor is provided with the kettle top of reactor, the fluid inlet of the injection reactor and reactant outlet are located at respectively two ends,
Gas phase entrance is located at the side of injection reactor；The feed being connected with injection reactor respectively is provided with the bottom of acyl chloride reaction kettle
Pump and reaction cycle pump.
The acyl chloride reaction kettle is additionally provided with acyl chlorides heat exchanger.
The acyl chloride reaction kettle is provided with remote liquid level instrument and online reaction mass analyser.By remote liquid level instrument and online
Reaction mass analyser carries out on-line analyses, liquid level and the conveying capacity of kettle and adjustment backward in control kettle to product in reactor
The intake of phosgene so that production is more precise and stable.
The acyl chloride reaction system includes six acyl chloride reaction kettles being sequentially connected in series.
Six acyl chloride reaction kettles be followed successively by No. 1 acyl chloride reaction kettle, No. 2 acyl chloride reaction kettles, No. 3 acyl chloride reaction kettles, No. 4
Acyl chloride reaction kettle, No. 5 acyl chloride reaction kettles and No. 6 acyl chloride reaction kettles, wherein the outlet of No. 6 acyl chloride reaction kettles and No. 1 acyl chloride reaction
The import of injection reactor in kettle is connected, the import of injection reactor in the outlet of No. 5 acyl chloride reaction kettles and No. 2 acyl chloride reaction kettles
It is connected, the outlet of No. 4 acyl chloride reaction kettles is connected with the import of injection reactor in No. 3 acyl chloride reaction kettles.The process units is adopted
The pattern of secondary response, substantially increases the yield of product, wherein No. 4 acyl chloride reaction kettles, No. 5 acyl chloride reaction kettles and No. 6 acyl chlorides
Reactor belongs to first order reaction, and yield is at least up to 71%；No. 1 acyl chloride reaction kettle, No. 2 acyl chloride reaction kettles and No. 3 acyl chloride reaction kettles
Belong to secondary response, yield can reach more than 84%.
The stearic purification system catches up with light kettle, acyl chlorides to catch up with light kettle to connect filter including acyl chlorides.
The filter includes grade one filter and secondary filter.
The exhaust treatment system includes glycerol absorption kettle, glycerol absorption kettle connection tail gas breaking plant.
Also include DCS automatic control systems.The automatic control system can carry out precise control to course of reaction and record
Temperature, liquid level, supplementary material flow so that reacting balance, eliminate error and deviation that manual operation brings, make product
Quality is more stable.
Also include the online thermometer of raw material and raw materials quality effusion meter.By the online thermometer of raw material and raw materials quality flow
Meter controls raw material dosage and adds speed, and maximum reaction rate improves purity, stability and the yield of product,
Reduce the yield of by-product.
The beneficial effects of the utility model are：The continuous production device of stearic described in the utility model is in acyl chlorides
Injection reactor is provided with the kettle top of reactor, gas phase phosgene is inhaled into the mixing of injection reactor and liquid phase stearic acid and DMF
Thing is reacted in injection reactor, and the device is designed to meet the contact surface area between gas-liquid two-phase, while contacting table
Constantly update in face so that the gas concentration that the gas-liquid two-phase on contact surface both sides remains sufficiently large is poor, improves chloride
Speed, on the basis of product quality is ensured, substantially reduces reaction time, improves production capacity.
Simultaneously thang-kng method is changed, injection reactor thang-kng is changed to by traditional bubbling thang-kng, increased phosgene hard
The time of staying in fat acid, the conversion ratio for making phosgene is improved, and reduces phosgene consumption, in a disguised form reduces the consumption of coke.Enter one
The consumption of yield and alkali liquor that step reduces by-product hydrochloric acid alleviates the load of exhaust treatment system.Simultaneous reactions stirring
Revocation, reduces the consumption of electric energy.
In sum, the process units adopts continuity method, various operating parameters to stablize, and farthest accelerates reaction speed
Rate, improves purity, stability and the yield of product, reduces the yield of by-product.
Description of the drawings
Fig. 1 is the structural representation of the continuous production device of stearic in this utility model specific embodiment.
Fig. 2 is the structural representation of injection reactor in this utility model specific embodiment
Wherein, 1 is acyl chloride reaction kettle, and 2 is injection reactor, and 3 is fluid inlet, and 4 are reactant outlet, and 5 enter for gas phase
Mouthful, 6 is feed pump, and 7 is reaction cycle pump, and 8 is acyl chlorides heat exchanger, and 9 catch up with light kettle for acyl chlorides, and 10 is grade one filter, and 11 is two
Level filter, 12 is glycerol absorption kettle.
Specific embodiment
Below in conjunction with the accompanying drawings, the technical solution of the utility model is described in detail.
It can be seen that the continuous production device of stearic described in the utility model, successively including acyl chlorides
Response system, stearic purification system and exhaust treatment system；The acyl chloride reaction system includes acyl chloride reaction kettle 1, should
Injection reactor 2 is provided with the kettle top of acyl chloride reaction kettle 1, the fluid inlet 3 of the injection reactor 2 and reactant outlet 4 are distinguished
Positioned at two ends, gas phase entrance 5 is located at the side of injection reactor 2；It is provided with the bottom of acyl chloride reaction kettle 1 and reacts with injection respectively
The connected feed pump 6 of device 2 and reaction cycle pump 7.
The acyl chloride reaction kettle 1 is additionally provided with acyl chlorides heat exchanger 8.
The acyl chloride reaction kettle 1 is provided with remote liquid level instrument and online reaction mass analyser.By remote liquid level instrument and
Line reaction mass analyser carries out on-line analyses to product in reactor, liquid level and the conveying capacity and tune of kettle backward in control kettle
The intake of whole phosgene so that production is more precise and stable.
The acyl chloride reaction system includes six acyl chloride reaction kettles 1 being sequentially connected in series.
Six acyl chloride reaction kettles 1 be followed successively by No. 1 acyl chloride reaction kettle, No. 2 acyl chloride reaction kettles, No. 3 acyl chloride reaction kettles, 4
Number acyl chloride reaction kettle, No. 5 acyl chloride reaction kettles and No. 6 acyl chloride reaction kettles, wherein the outlet of No. 6 acyl chloride reaction kettles is anti-with No. 1 acyl chlorides
The import for answering injection reactor in kettle is connected, and the outlet of No. 5 acyl chloride reaction kettles is entered with injection reactor in No. 2 acyl chloride reaction kettles
Mouth is connected, and the outlet of No. 4 acyl chloride reaction kettles is connected with the import of injection reactor in No. 3 acyl chloride reaction kettles.The process units is adopted
With the pattern of secondary response, the yield of product is substantially increased, wherein No. 4 acyl chloride reaction kettles, No. 5 acyl chloride reaction kettles and No. 6 acyls
Chlorine reactor belongs to first order reaction, and yield is at least up to 71%；No. 1 acyl chloride reaction kettle, No. 2 acyl chloride reaction kettles and No. 3 acyl chloride reactions
Kettle belongs to secondary response, and yield can reach more than 84%.
The stearic purification system catches up with light kettle 9, acyl chlorides to catch up with light kettle 9 to connect filter including acyl chlorides.
The filter includes grade one filter 10 and secondary filter 11.
The exhaust treatment system includes glycerol absorption kettle 12, the connection tail gas breaking plant of glycerol absorption kettle 12.
Also include DCS automatic control systems.The automatic control system can carry out precise control to course of reaction and record
Temperature, liquid level, supplementary material flow so that reacting balance, eliminate error and deviation that manual operation brings, make product
Quality is more stable.
Also include the online thermometer of raw material and raw materials quality effusion meter.By the online thermometer of raw material and raw materials quality flow
Meter controls raw material dosage and adds speed, and maximum reaction rate improves purity, stability and the yield of product,
Reduce the yield of by-product.
The device carries out continuous prodution reaction unit using injection reactor, from the stearic acid Jing raw materials quality of tank field
Effusion meter and DMF enter No. 1 acyl chloride reaction kettle after mixing in proportion, then according to remote liquid level instrument and online reaction mass
The measurement monitoring of analyser pumps into successively No. 2, No. 3, No. 4, No. 5 and No. 6 acyl chloride reaction kettles, and course of reaction is that two-stage chloride is anti-
Should, fresh phosgene by injection reactor respectively enter No. 4, No. 5, No. 6 acyl chloride reaction kettles carry out one-level acyl chloride reaction, one-level
Reacted tail gas corresponds to respectively Jing injection reactors and carries out two grades of acyl chloride reactions into No. 3, No. 2, No. 1 acyl chloride reaction kettle,
The crude product stearyl chloride that No. 6 acyl chloride reaction kettles of Jing are pumped out is continuously entered catches up with light kettle to catch up with light and activated carbon decolorizing, it is qualified after Jing mono-,
After secondary filter is filtered, obtain product stearyl chloride and enter product storage tank；It is sweet that acyl chloride reaction tail gas house steward Jing enters I and II
Oily absorption kettle can be with catching up with light tail gas to carry out tail gas destruction operation into tail gas breaking plant after absorbing, and glycerol absorbs gained dichloro third
Alcohol pumps into ECH workshops.
Stearic acid and DMF enter injection reactor by feed pump via the fluid inlet of injection reactor, and phosgene is by gas
Phase entrance is sucked, and liquid phase carries out being sufficiently mixed reaction in injection reactor, and reactant flows out via reactant outlet injection,
The main component that reactant outlet injection is flowed out includes stearyl chloride, a small amount of stearic acid and a small amount of unreacted phosgene, reaction tail
Gas and catalyst etc..
Claims (10)
1. a kind of continuous production device of stearic, successively including acyl chloride reaction system, stearic purification system
And exhaust treatment system；Characterized in that, the acyl chloride reaction system includes acyl chloride reaction kettle, at the kettle top of the acyl chloride reaction kettle
Injection reactor is provided with, the fluid inlet of the injection reactor and reactant outlet are located at respectively two ends, and gas phase entrance is located at spray
Penetrate the side of reactor；The feed pump and reaction cycle being connected with injection reactor respectively is provided with the bottom of acyl chloride reaction kettle
Pump.
2. the continuous production device of stearic according to claim 1, it is characterised in that the acyl chloride reaction kettle is also
It is provided with acyl chlorides heat exchanger.
3. the continuous production device of stearic according to claim 1, it is characterised in that the acyl chloride reaction kettle sets
There are remote liquid level instrument and online reaction mass analyser.
4. the continuous production device of stearic according to claim 1, it is characterised in that the acyl chloride reaction system
Including six acyl chloride reaction kettles being sequentially connected in series.
5. the continuous production device of stearic according to claim 4, it is characterised in that six acyl chloride reactions
Kettle is followed successively by No. 1 acyl chloride reaction kettle, No. 2 acyl chloride reaction kettles, No. 3 acyl chloride reaction kettles, No. 4 acyl chloride reaction kettles, No. 5 acyl chloride reaction kettles
With No. 6 acyl chloride reaction kettles, wherein the outlet of No. 6 acyl chloride reaction kettles is connected with the import of injection reactor in No. 1 acyl chloride reaction kettle,
The outlet of No. 5 acyl chloride reaction kettles is connected with the import of injection reactor in No. 2 acyl chloride reaction kettles, the outlet of No. 4 acyl chloride reaction kettles
It is connected with the import of injection reactor in No. 3 acyl chloride reaction kettles.
6. the continuous production device of stearic according to claim 1, it is characterised in that the stearic is pure
Change system catches up with light kettle, acyl chlorides to catch up with light kettle to connect filter including acyl chlorides.
7. the continuous production device of stearic according to claim 6, it is characterised in that the filter includes
Level filter and secondary filter.
8. the continuous production device of stearic according to claim 1, it is characterised in that the exhaust treatment system
Including glycerol absorption kettle, glycerol absorption kettle connection tail gas breaking plant.
9. the continuous production device of stearic according to claim 1, it is characterised in that also control automatically including DCS
System processed.
10. the continuous production device of stearic according to claim 1, it is characterised in that also online including raw material
Thermometer and raw materials quality effusion meter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621131150.7U CN206173250U (en) | 2016-10-18 | 2016-10-18 | Serialization apparatus for producing of stearic acid acyl chlorides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621131150.7U CN206173250U (en) | 2016-10-18 | 2016-10-18 | Serialization apparatus for producing of stearic acid acyl chlorides |
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| Publication Number | Publication Date |
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| CN206173250U true CN206173250U (en) | 2017-05-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201621131150.7U Active CN206173250U (en) | 2016-10-18 | 2016-10-18 | Serialization apparatus for producing of stearic acid acyl chlorides |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111454147A (en) * | 2020-05-06 | 2020-07-28 | 山东博宏新化工科技有限公司 | Treatment process and equipment for hazardous waste activated carbon for production of stearic acid acyl chloride |
| CN115894244A (en) * | 2022-09-26 | 2023-04-04 | 湖南化工研究院有限公司 | Continuous synthesis method of isopropyl chloride |
-
2016
- 2016-10-18 CN CN201621131150.7U patent/CN206173250U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111454147A (en) * | 2020-05-06 | 2020-07-28 | 山东博宏新化工科技有限公司 | Treatment process and equipment for hazardous waste activated carbon for production of stearic acid acyl chloride |
| CN115894244A (en) * | 2022-09-26 | 2023-04-04 | 湖南化工研究院有限公司 | Continuous synthesis method of isopropyl chloride |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20181026 Address after: 272117 middle section of Yanan Road, Yanzhou District, Jining, Shandong. Patentee after: Camilla Tiancheng Wanfeng chemicals (Yanzhou) Co., Ltd. Address before: 272117 No. 66 North Station West Road, Yanzhou District, Jining, Shandong. Patentee before: Shandong Tiancheng Wanfeng Chemical Technology Co., Ltd. |