CN203021485U - System for continuously producing ethyl butyrate - Google Patents
System for continuously producing ethyl butyrate Download PDFInfo
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- CN203021485U CN203021485U CN 201320001627 CN201320001627U CN203021485U CN 203021485 U CN203021485 U CN 203021485U CN 201320001627 CN201320001627 CN 201320001627 CN 201320001627 U CN201320001627 U CN 201320001627U CN 203021485 U CN203021485 U CN 203021485U
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Abstract
The utility model discloses a system for continuously producing ethyl butyrate, which consists of a feed system, a reaction system and a separation system, wherein the feed system comprises a butyric acid raw material tank, an ethanol raw material tank and a metering pump; the reaction system comprises a mixer, a reactor, a solid catalyst, a crude product tank and a metering pump; and the separation system comprises a first-level classification tower, an oil-water separator, a second-level dealcoholization tower, a third-level finished product tower and a metering pump. The system disclosed by the utility model realizes continuous production of ethyl butyrate through continuous mixing and dosing, feed reaction and three-section rectifying separation.
Description
Technical field
The utility model relates to a kind of system of continuous production chemical product, particularly a kind of system of continuous production ethyl butyrate.
Background technology
Produce at present ethyl butyrate, generally adopt interrupter method, take butanic acid, ethanol as raw material, take sulfuric acid or tosic acid etc. as catalyzer, take hexanaphthene, benzene or toluene as the band aqua, employing is with the reactor of division box, the reacting by heating still carries out esterification, adopts continuously water, until reaction finishes, through cooling, neutralization, washing, then separate obtaining finished product again.Process flow sheet is as follows:
This production technique periodical operation, efficient is lower, and catalyzer can not reuse, and neutralization, washing all exist certain loss of material and three-waste pollution problem, and recovered material also needs energy consumption.And take sulfuric acid etc. as catalyzer, by product is more, equipment corrosion is serious.
The green catalysis technology is to realize the Main Means of chemical production processes greenization, and in recent years, at Field of Fine Chemicals, how replacing original pollution poor efficiency technique with the heterogeneous catalysis technology of green non-pollution has become an important research direction.
Summary of the invention
But technical problem to be solved in the utility model is to provide a kind of continuous feeding and discharging, successive reaction, continuous separate from the system of, production efficiency is high, technique is green continuous production ethyl butyrate.
the utility model provides following technical scheme in order to solve above-mentioned technical problem: a kind of system of continuous production ethyl butyrate, it is characterized in that comprising feed system, reactive system, separation system, and feed system comprises butyric acid head tank, ethanol raw material tank, described reactive system comprises mixing tank, reactor, thick products pot, described separation system comprises one-level classification tower, water-and-oil separator, secondary dealcoholize column and three grades of finishing columns, described butyric acid head tank, ethanol raw material tank pipeline connects mixing tank, mixing tank pipeline ligation device bottom opening for feed, in described reactor, solid catalyst is housed, reactor upper end discharge opening pipeline connects thick products pot, thick products pot pipeline connection one-level classification tower middle and lower part opening for feed, one-level classification column overhead is provided with reflux line and connects mixing tank, one-level classification tower tower reactor is provided with pipeline and connects mixing tank, one-level classification tower middle and upper part is provided with discharge opening pipeline and connects water-and-oil separator, water-and-oil separator pipeline connection secondary dealcoholize column middle and upper part opening for feed, secondary dealcoholize column top pipeline connects mixing tank, secondary dealcoholize column tower reactor discharge opening pipeline connects three grades of finishing column tower reactor opening for feeds, described three grades of finishing column tower tops are provided with discharge pipe.
Be provided with volume pump on described butyric acid head tank, ethanol raw material tank and pipeline that mixing tank is connected.
Be provided with volume pump on described mixing tank and pipeline that reactor bottom opening for feed is connected.
Be provided with volume pump on the opening for feed connecting tube of described thick products pot and one-level classification tower middle and lower part.
Be provided with volume pump on described water-and-oil separator and secondary dealcoholize column middle and upper part opening for feed connecting tube.
Be provided with volume pump on described secondary dealcoholize column tower reactor discharge port and three grades of finishing column tower reactor opening for feed connecting tubes.
Preferred as the utility model, described solid catalyst is (by force) acidic resins, heteropolyacid, zirconium sulfate or molecular sieve.By adopting solid catalyst, effectively prevented from utilizing in prior art the strong acidic liquid catalyzer such as sulfuric acid to cause equipment corrosion, shorten work-ing life, and be easy to separate reusable, the most important thing is to prevent that liquid catalyst and raw material butyric acid and ethanol from reacting, the by product that output is unnecessary affects production efficiency and is difficult to and processes.
As further improvement of the utility model, described reactor is provided with temperature control unit.Control the temperature of reaction of reactor by this temperature control unit.
For better explaining the technical solution of the utility model, below introduce in detail principle of work of the present utility model: with raw material butyric acid and ethanol, be continuously pumped into mixing tank by volume pump respectively, mixed raw material passes into continuously catalytic unit is housed, with carrying out esterification in the reactor of temperature regulating device, opening for feed is positioned at the reactor bottom, discharge port is positioned at the reactor upper end, and the thick product continuous discharge of generation buffers in thick product storage tank, and this storage tank is furnished with blow-down pipe and keeps normal pressure.Then thick product is continuously pumped into one-level classification tower by volume pump and classifies, opening for feed is positioned at one-level classification tower body middle and lower part, unreacted ethanol returns to mixing tank from the continuous extraction of one-level classification column overhead, unreacted butyric acid also returns to mixing tank from one-level classification tower tower reactor continuous discharge, the ethyl butyrate that generates and water separate through water-and-oil separator from being positioned at the continuous extraction of discharge port of one-level classification tower tower body middle and upper part.Generate the organism qualified discharge after the processing such as recovery of necessity in water, it is very high that the ethyl butyrate oil reservoir contains the ester amount, be continuously pumped into the secondary dealcoholize column by volume pump and remove a small amount of second alcohol and water, opening for feed is positioned at the tower body middle and upper part, a small amount of aqueous ethanol is from overhead extraction, return to mixing tank, secondary dealcoholize column tower reactor continuous discharge also directly pumps into three grades of finishing column tower reactors, at last continuously from finishing column overhead extraction ethyl butyrate finished product.
In described technical scheme, the solid catalyst that loads in reactor can be (by force) acidic resins, heteropolyacid, zirconium sulfate or molecular sieve etc.One-level classification tower, secondary dealcoholize column, three grades of finishing columns are all the rectifying tower that is filled with stainless steel or magnet ring, and each rectifying tower provides power by the Boiler Steam heating.
The beneficial effects of the utility model: the utility model adopts solid catalyst and heterogeneous reaction technique thereof to substitute traditional homogeneous catalysis technique, and major advantage is that catalyzer is easy to separate, and is reusable, less pollution, make more greenization of technique, and can realize serialization production, efficient is high.
Description of drawings
Fig. 1 is system construction drawing of the present utility model.
Embodiment
a kind of system of continuous production ethyl butyrate comprises feed system, reactive system, separation system, and feed system comprises butyric acid head tank 001, ethanol raw material tank 002, described reactive system comprises mixing tank 003, reactor 004, thick products pot 005, described separation system comprises one-level classification tower 006, water-and-oil separator 007, secondary dealcoholize column 008 and three grades of finishing columns 009, described butyric acid head tank 001, ethanol raw material tank 002 pipeline connects mixing tank 003, mixing tank 003 pipeline ligation device 004 bottom opening for feed, in described reactor 004, solid catalyst 041 is housed, reactor 004 upper end discharge opening pipeline connects thick products pot 005, thick products pot 005 pipeline connects one-level classification tower 006 middle and lower part opening for feed, one-level classification tower tower 006 top is provided with reflux line and connects mixing tank 003, one-level classification tower 006 tower reactor 061 is provided with pipeline and connects mixing tank 003, one-level classification tower 006 middle and upper part is provided with discharge opening pipeline and connects water-and-oil separator 007, water-and-oil separator 007 pipeline connects secondary dealcoholize column 008 middle and upper part opening for feed, secondary dealcoholize column 008 top pipeline connects mixing tank 003, secondary dealcoholize column 008 tower reactor 081 discharge opening pipeline connects three grades of finishing column 009 tower reactor 091 opening for feeds, described three grades of finishing column 009 tower tops are provided with discharge pipe, described butyric acid head tank 001, be provided with volume pump 010 on ethanol raw material tank 002 and pipeline that mixing tank 003 is connected, be provided with volume pump 010 on described mixing tank 003 and pipeline that reactor 004 bottom opening for feed is connected, be provided with volume pump 010 on described thick products pot 005 and one-level classification tower 006 middle and lower part opening for feed connecting tube, be provided with volume pump 010 on described water-and-oil separator 007 and secondary dealcoholize column 008 middle and upper part opening for feed connecting tube, be provided with volume pump 010 on described secondary dealcoholize column 008 tower reactor 081 discharge port and three grades of finishing column 009 tower reactor 091 opening for feed connecting tubes, preferred as the utility model, described solid catalyst 041 is (by force) acidic resins, heteropolyacid, zirconium sulfate or molecular sieve.Described reactor is provided with temperature control unit.
Be more than basic embodiment of the present utility model, below introduce in detail the utility model specific embodiment.
embodiment 1: as shown in Figure 1, the interior filling 3500 kg highly acidic resins of reactor 004 are catalyzer, before starting the continuous feeding and discharging reaction, it is first the reactor 004 of 5 cubic metres with the raw material butyric acid of equimolar ratio and the full volume of ethanol storage, reactor 004 temperature is controlled at 75 ℃, question response is during to equilibrium conversion (esterification yield approximately 45%), and then restart charging volume pump 010, this moment, the input speed of butyric acid was 384 kg/h, the input speed of ethanol is 200 kg/h, fresh feed is after mixing tank 003 mixes, pass into continuously reactor 004 by reactor 004 bottom entrance, the thick product of simultaneous reactions is by reactor 004 top outlet continuous discharge, discharge port is normal pressure, this moment, discharging speed was 584 kg/h, suitable with input speed, in reactor 004, material is full state.
The thick product continuous discharge that generates buffers in thick product storage tank 005, and this storage tank 005 is furnished with blow-down pipe to keep normal pressure.
then thick product is continuously pumped into one-level classification tower 006 by volume pump 010 and classifies, provide power by Boiler Steam, inlet amount is 584 kg/h, suitable with reactor 004 input and output material amount, opening for feed is positioned at one-level classification tower 006 tower body middle and lower part, unreacted ethanol directly returns to mixing tank 003 from the continuous extraction of tower top, ethanol content 95% is adopted on the top, another moisture 5%, it is 108 kg/h that the top is adopted with retum speed, quantity of reflux is 360 kg/h, unreacted butyric acid also returns to mixing tank 003 from one-level classification tower 006 tower reactor 061 continuous discharge, tower reactor 061 goes out butyric acid content up to 99% left and right, retum speed is 196 kg/h.At this moment, the input speed of fresh butyric acid is adjusted into 192 kg/h and is settled out by 384 kg/h, the input speed of fresh ethanol is adjusted into 100 kg/h and is settled out by 200 kg/h, fresh feed and separation system are returned to unreacted butyric acid and ethanol after mixing tank 003 mixes, same continuously feeding reaction.
the ethyl butyrate that generates and water are from being positioned at the continuous extraction of discharge port of one-level classification tower 006 tower body middle and upper part, through water-and-oil separator 007 separately, be dissolved with minute quantity ethanol in water, the organism such as ethyl butyrate, qualified discharge after the recycling of necessity, ethyl butyrate oil reservoir ester content 96%, mainly contain in addition a small amount of second alcohol and water, it is continuously pumped into secondary dealcoholize column 008 by volume pump 010, the second alcohol and water is removed, opening for feed is positioned in the middle part of secondary dealcoholize column 008 tower body, input speed is 260 kg/h, a small amount of aqueous ethanol is from secondary dealcoholize column 008 overhead extraction, the a small amount of ethyl butyrate of extraction simultaneously, directly return to mixing tank 003, rate of yield is 20 kg/h, quantity of reflux is 250 kg/h, in secondary dealcoholize column 008 tower reactor 081, ethyl butyrate content is more than 99%, continuous discharge also directly pumps into three grades of finishing columns, 009 tower reactor 091, last is 99.8% finished product continuously from finishing column 009 overhead extraction ethyl butyrate content, the finished product rate of yield is 240 kg/h, quantity of reflux is 360 kg/h.
Claims (8)
1. a system that produces continuously ethyl butyrate, is characterized in that comprising feed system, reactive system, separation system, and feed system comprises butyric acid head tank, ethanol raw material tank, described reactive system comprises mixing tank, reactor, thick products pot, described separation system comprises one-level classification tower, water-and-oil separator, secondary dealcoholize column and three grades of finishing columns, described butyric acid head tank, ethanol raw material tank pipeline connects mixing tank, mixing tank pipeline ligation device bottom opening for feed, in described reactor, solid catalyst is housed, reactor upper end discharge opening pipeline connects thick products pot, thick products pot pipeline connection one-level classification tower middle and lower part opening for feed, one-level classification column overhead is provided with reflux line and connects mixing tank, one-level classification tower tower reactor is provided with pipeline and connects mixing tank, one-level classification tower middle and upper part is provided with discharge opening pipeline and connects water-and-oil separator, water-and-oil separator pipeline connection secondary dealcoholize column middle and upper part opening for feed, secondary dealcoholize column top pipeline connects mixing tank, secondary dealcoholize column tower reactor discharge opening pipeline connects three grades of finishing column tower reactor opening for feeds, described three grades of finishing column tower tops are provided with discharge pipe.
2. the system of a kind of continuous production ethyl butyrate according to claim 1 is characterized in that being provided with volume pump on described butyric acid head tank, ethanol raw material tank and pipeline that mixing tank is connected.
3. the system of a kind of continuous production ethyl butyrate according to claim 1 is characterized in that being provided with volume pump on described mixing tank and pipeline that reactor bottom opening for feed is connected.
4. the system of a kind of continuous production ethyl butyrate according to claim 1 is characterized in that being provided with volume pump on the opening for feed connecting pipeline of described thick products pot pipeline and one-level classification tower middle and lower part.
5. the system of a kind of continuous production ethyl butyrate according to claim 1 is characterized in that being provided with volume pump on described water-and-oil separator and secondary dealcoholize column middle and upper part opening for feed connecting tube.
6. the system of a kind of continuous production ethyl butyrate according to claim 1, is characterized in that being provided with volume pump on described secondary dealcoholize column tower reactor discharge port and three grades of finishing column tower reactor opening for feed connecting tubes.
7. the system of a kind of continuous production ethyl butyrate according to claim 1, is characterized in that described solid catalyst is (by force) acidic resins, heteropolyacid, zirconium sulfate or molecular sieve.
8. the system of a kind of continuous production ethyl butyrate according to claim 1, is characterized in that described reactor is provided with temperature control unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320001627 CN203021485U (en) | 2013-01-04 | 2013-01-04 | System for continuously producing ethyl butyrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320001627 CN203021485U (en) | 2013-01-04 | 2013-01-04 | System for continuously producing ethyl butyrate |
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| CN203021485U true CN203021485U (en) | 2013-06-26 |
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| CN 201320001627 Expired - Lifetime CN203021485U (en) | 2013-01-04 | 2013-01-04 | System for continuously producing ethyl butyrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058860A (en) * | 2013-01-04 | 2013-04-24 | 宜兴市恒兴精细化工有限公司 | System for producing ethyl butyrate continuously |
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2013
- 2013-01-04 CN CN 201320001627 patent/CN203021485U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058860A (en) * | 2013-01-04 | 2013-04-24 | 宜兴市恒兴精细化工有限公司 | System for producing ethyl butyrate continuously |
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| C14 | Grant of patent or utility model | ||
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Address after: 214213 Yongning Branch Road, Yixing Economic and Technological Development Zone, Wuxi City, Jiangsu Province Patentee after: Jiangsu Hengxing New Material Technology Co.,Ltd. Address before: 214213 Yongning Road, Yixing Economic Development Zone, Wuxi, Jiangsu Patentee before: YIXING HENGXING FINE CHEMICAL Co.,Ltd. |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130626 |