CN204454715U - A kind of triethylamine retrieving arrangement - Google Patents
A kind of triethylamine retrieving arrangement Download PDFInfo
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- CN204454715U CN204454715U CN201520053744.XU CN201520053744U CN204454715U CN 204454715 U CN204454715 U CN 204454715U CN 201520053744 U CN201520053744 U CN 201520053744U CN 204454715 U CN204454715 U CN 204454715U
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- triethylamine
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Abstract
The utility model relates to a kind of triethylamine retrieving arrangement, is mainly used in reclaiming triethylamine from triethylamine hydrochloride waste water, belongs to chemical wastewater treatment technical field.Solve traditional device recovery triethylamine yield low, reclaim the moisture higher technical problem of triethylamine.Retrieving arrangement of the present utility model, utilizes the temperature of the water management removal process of room temperature at 20 ~ 30 DEG C, avoids triethylamine and water to dissolve each other, and volatilization loss; Utilize salting-out effect, reduce the solubleness of triethylamine in water; In delaminating process, oil reservoir separates from layering visor top, and delaminating process loses without oil reservoir.These measures make the triethylamine rate of recovery bring up to more than 95%, are moisturely down to less than 1%.Retrieving arrangement of the present utility model, closed-loop operation, process safety, cost recovery is cheap, reclaims triethylamine and conveniently applies mechanically, Suitable commercial adopts.
Description
Technical field
The utility model relates to triethylamine retrieving arrangement, is mainly used in reclaiming triethylamine from triethylamine hydrochloride waste water, belongs to chemical wastewater treatment technical field.
Background technology
Triethylamine, structural formula (C
2h
5)
3n.Colourless or light yellow transparent liquid, has smelly ammonia taste.Boiling point 89.5 DEG C.Time below 18.7 DEG C, can be miscible with water, more than this temperature, be only slightly soluble in water.There is the chemical property of tertiary amine, in alkalescence.To skin and mucous membrane irritation strong.
Triethylamine is in the acylation reaction of acyl chlorides (carbonyl chloride, phosphoryl chloride, SULPHURYL CHLORIDE); be widely used as acid binding agent---the trapping agent of hydrogenchloride; reaction generates solid by-product triethylamine hydrochloride; the latter is soluble in water; aftertreatment adopts water extraction, obtains the waste water containing triethylamine hydrochloride.
Triethylamine price is more expensive and toxicity is higher, reclaims triethylamine apply mechanically from containing the waste water of triethylamine hydrochloride, for conservation, reduce Toxic waste discharge, protection of the environment is significant.
From triethylamine hydrochloride, reclaim triethylamine, adopt the method that triethylamine dissociates out by sodium hydroxide and triethylamine hydrochloride effect at large, reaction formula is shown in (1), obtains triethylamine after separate aqueous layer.
(C
2H
5)
3N·HCl+NaOH＝(C
2H
5)
3N+NaCl+H
2O (1)
Traditional retrieving arrangement; do not control to reclaim the concentration of sodium chloride salt in the temperature of reaction and water layer; due to triethylamine volatilization or in water solubleness larger; cause the rate of recovery lower (60% ~ 85%); moisture higher (1% ~ 3%), can not overlap for the acylation reaction higher to moisture requirement.
Summary of the invention
Technical problem to be solved in the utility model is: develop a kind of triethylamine retrieving arrangement, and the shortcoming overcoming traditional retrieving arrangement, with not enough, improve the rate of recovery of triethylamine, reduces the water content reclaimed in triethylamine.
For solving the problems of the technologies described above, the technical solution of the utility model is:
A kind of triethylamine retrieving arrangement, comprises and reclaims still 1, agitator 2, chuck 3, thermometer 4, layering visor 5.
Discharge port bottom described recovery still 1 connects bleeder valve 7, threeway 21, layering visor 5, shunt valve 6, waste pipe 22 successively, and the side mouth of threeway 21 connects recovery amine pipe 20 by point amine valve 19.
The stirring port of described recovery still 1 top center is provided with agitator 2, the temperature-measuring port at top is inserted with thermowell 18, thermometer 4 is inserted with in thermowell 18, the amine salt mouth of a river at top connects amine salt water pipe 11 by amine salt water valve 10, the concentrated base mouth at top connects concentrated base pipe 12 by concentrated base valve 13, and the drain at top connects blow-down pipe 15 by blow-off valve 14.
Described recovery still 1 outside is provided with chuck 3, and the water-in bottom chuck connects water inlet pipe 9 by water intaking valve 8, and the water outlet on chuck top connects rising pipe 16 by outlet valve 17.
Recovery still 1 of the present utility model, inside is provided with agitator 2, thermometer 4 (being placed in thermowell 18), and outside is provided with chuck 3, and bottom is provided with layering visor 5.Agitator 2, for making reaction mixture even, fully reacts, does not stay dead angle; Thermometer 4 is for monitoring the temperature of removal process, and it is to be protected that thermometer 4 is placed in thermowell 18, in case dielectric corrosion measures inaccurate or is subject to damage of colliding with; Water flowing in chuck, for controlling the temperature of removal process within the scope of 20 ~ 30 DEG C, in temperature lower than 18.7 DEG C, triethylamine and the miscible water content that causes of water section increase, and in temperature higher than 30 DEG C, triethylamine volatilization causes the rate of recovery to decline; Layering visor 5 for separating of water layer, and is used as flow view.
Mode of connection bottom recovery still 1 of the present utility model is the water layer in order to separate lower floor, reclaims the oil reservoir triethylamine on upper strata.Dividing amine valve 19, reclaim the top that amine pipe 20 is arranged on layering visor 5, is in order to avoid reclaiming triethylamine mechanical entrapment moisture, reducing the water content reclaiming triethylamine.When dividing water-yielding stratum to water-oil interface to occur in layering visor 5, stopping a point water, starting to separate triethylamine to flowing out without triethylamine.Comprise layering visor 5, a small amount of oil reservoir retained in the pipeline below shunt valve more than 6 to the side mouth of threeway 21 and water layer, temporarily exist wherein, give over to merge with next batch and be separated, triethylamine can not be caused to lose.
The top of recovery still 1 of the present utility model, is at least provided with 5 mouths, is stirring port, temperature-measuring port, the amine salt mouth of a river, concentrated base mouth, drain respectively.Stirring port is located at center, and be beneficial to and install agitator 2, and make to stir, other mouthfuls are located at around stirring port.Temperature-measuring port installs thermowell 18 by Flange joint, and thermometer 4 inserts wherein, can drip glycerine and be beneficial to thermometric in the bottom of thermowell 18.The amine salt mouth of a river and concentrated base mouth are all liquid inlet openings, these two opening for feeds can merge and utilize an opening for feed, another opening for feed vacateed is as mouth for subsequent use, (triethylamine hydrochloride or liquid caustic soda concentration lower) is for adding alkali, the salt of solid where necessary, make aqueous phase saturated or intimate saturated, utilize salting-out effect like this, reduce triethylamine solubleness in water, improve the rate of recovery of triethylamine.The triethylamine hydrochloride waste water of liquid and concentrated base, by pumping, potential difference, vacuum, manually the mode such as to pour into and feed in raw material; Alkali, the salt of solid are fed in raw material by machinery or mode of manually pouring into.Drain connects exhausting pipeline, and for making recovery still 1 keep atmospheric pressure state, if adopt vacuum charging, drain can be the two-in-one mouth of pipe of vacuum and emptying.
The chuck 3 of recovery still 1 outside of the present utility model, leakes water in the mode of " bottom in and top out ", can guarantee to be full of water in chuck, be beneficial to heat transfer.Water can be tap water or the recirculated water of room temperature.It is thermopositive reaction that triethylamine hydrochloride and sodium hydroxide react, and utilizes the water cooling of room temperature can prevent temperature from raising and causes triethylamine volatilization loss.Separately, if temperature of reaction system is lower than room temperature, the water of room temperature just plays heat effect, can prevent triethylamine and water section miscible, cause water content to increase.The water of room temperature is utilized to make cold and hot matchmaker or refrigerant, conserve energy.
The beneficial effects of the utility model are: the temperature controlling removal process, and utilize salting-out effect, delaminating process is guaranteed to lose without oil reservoir, the triethylamine rate of recovery is made to bring up to more than 95%, moisturely be down to 0.5% ~ 1%, cost recovery is cheap, reclaims triethylamine and conveniently applies mechanically.
Below in conjunction with drawings and embodiments, the utility model is described in further detail.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of triethylamine retrieving arrangement of the present utility model.
In figure: 1, reclaim still, 2, agitator, 3, chuck, 4, thermometer, 5, layering visor, 6, shunt valve, 7, bleeder valve, 8, water intaking valve, 9, water inlet pipe, 10, amine salt water valve, 11, amine salt water pipe, 12, concentrated base pipe, 13, concentrated base valve, 14, blow-off valve, 15, blow-down pipe, 16, rising pipe, 17, outlet valve, 18, thermowell, 19, point amine valve, 20, amine pipe is reclaimed, 21, threeway, 22, waste pipe.
Embodiment
Triethylamine retrieving arrangement shown in Fig. 1, comprises the recovery still 1 that volume is 5L, the low-speed agitator 2 matched, chuck 3, thermal resistance thermometer 4, and the layering visor 5 of glass tubular type.
Discharge port bottom described recovery still 1 connects bleeder valve 7, threeway 21, layering visor 5, shunt valve 6, waste pipe 22 successively, and the side mouth of threeway 21 connects recovery amine pipe 20 by point amine valve 19.
The stirring port of described recovery still 1 top center is provided with the low-speed anchor stirrer 2 of mechanical seal, the temperature-measuring port at top is provided with the thermowell 18 of Flange joint, glycerine is instilled bottom thermowell 18, insert the thermal resistance thermometer 4 of range-20 ~ 100 DEG C, the amine salt mouth of a river at top connects amine salt water pipe 11 by amine salt water valve 10, the concentrated base mouth at top connects concentrated base pipe 12 by concentrated base valve 13, and the drain at top connects blow-down pipe 15 by blow-off valve 14.
Described recovery still 1 outside is provided with chuck 3, and the water-in bottom chuck connects water inlet pipe 9 by water intaking valve 8, and the water outlet on chuck top connects rising pipe 16 by outlet valve 17.
The method of described triethylamine retrieving arrangement operation is as follows:
(1) reinforced: to open blow-off valve 14, make recovery still 1 keep atmospheric pressure state; Open water intaking valve 8, outlet valve 17, in chuck 3, pass into the recirculated water of 15 ~ 30 DEG C; Open amine salt water valve 10, added the triethylamine hydrochloride waste water 3kg of concentration 56% by amine salt water pipe 11, finish, close amine salt water valve 10; Start agitator 2; Open concentrated base valve 13, added the dope alkali 1.1kg of concentration 45% by concentrated base pipe 12, control the aperture of concentrated base valve 13 and water intaking valve 8 in the process, the temperature that thermometer 4 is shown maintains 20 ~ 30 DEG C, adds alkali complete, closes concentrated base valve 13.
(2) divide water: add alkali complete, continue to stir 10min, stop agitator 2, leave standstill 30min, open bleeder valve 7, slowly open shunt valve 6, water layer is released by waste pipe 22, when there is phase interface in layering visor 5, close shunt valve 6, water layer is separated and terminates.
(3) receive amine: open a point amine valve 19, by reclaiming amine pipe 20, triethylamine being put into container containing, reclaiming triethylamine moisture 0.9%, quantity 1.175kg, the rate of recovery 95.2%.Receipts amine is complete, closes point amine valve 19, a bleeder valve 7, retains a small amount of triethylamine and waste water, temporarily seal up for safekeeping wherein, give over to and merge layered shaping with next batch in the pipeline between the mouth of shunt valve 6 to threeway 21 side.
Claims (1)
1. a triethylamine retrieving arrangement, is characterized in that this device comprises and reclaims still (1), agitator (2), chuck (3), thermometer (4), layering visor (5); The discharge port of described recovery still (1) bottom connects bleeder valve (7), threeway (21), layering visor (5), shunt valve (6), waste pipe (22) successively, and the side mouth of threeway (21) connects recovery amine pipe (20) by point amine valve (19); The stirring port of described recovery still (1) top center is provided with agitator (2), the temperature-measuring port at top is provided with thermowell (18), thermometer (4) is inserted with in thermowell (18), the amine salt mouth of a river at top connects amine salt water pipe (11) by amine salt water valve (10), the concentrated base mouth at top connects concentrated base pipe (12) by concentrated base valve (13), and the drain at top connects blow-down pipe (15) by blow-off valve (14); Described recovery still (1) outside is provided with chuck (3), water-in bottom chuck connects water inlet pipe (9) by water intaking valve (8), and the water outlet on chuck top connects rising pipe (16) by outlet valve (17).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520053744.XU CN204454715U (en) | 2015-01-27 | 2015-01-27 | A kind of triethylamine retrieving arrangement |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520053744.XU CN204454715U (en) | 2015-01-27 | 2015-01-27 | A kind of triethylamine retrieving arrangement |
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| CN204454715U true CN204454715U (en) | 2015-07-08 |
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| CN201520053744.XU Expired - Fee Related CN204454715U (en) | 2015-01-27 | 2015-01-27 | A kind of triethylamine retrieving arrangement |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977409A (en) * | 2017-05-09 | 2017-07-25 | 浙江台州市联创环保科技有限公司 | A kind of separation method of triethylamine and water |
| CN109053627A (en) * | 2018-08-13 | 2018-12-21 | 国药集团威奇达药业有限公司 | The comprehensive recovering process of 2-mercaptobenzothiazole, triethylamine and methylene chloride in Ceftriaxone Sodium methylene chloride mother liquor |
| CN114560777A (en) * | 2022-02-24 | 2022-05-31 | 宁夏天霖新材料科技有限公司 | Continuous recovery method of triethylamine in VC production |
-
2015
- 2015-01-27 CN CN201520053744.XU patent/CN204454715U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977409A (en) * | 2017-05-09 | 2017-07-25 | 浙江台州市联创环保科技有限公司 | A kind of separation method of triethylamine and water |
| CN109053627A (en) * | 2018-08-13 | 2018-12-21 | 国药集团威奇达药业有限公司 | The comprehensive recovering process of 2-mercaptobenzothiazole, triethylamine and methylene chloride in Ceftriaxone Sodium methylene chloride mother liquor |
| CN109053627B (en) * | 2018-08-13 | 2020-11-06 | 国药集团威奇达药业有限公司 | Comprehensive recovery method of 2-mercaptobenzothiazole, triethylamine and dichloromethane in ceftriaxone sodium dichloromethane mother liquor |
| CN114560777A (en) * | 2022-02-24 | 2022-05-31 | 宁夏天霖新材料科技有限公司 | Continuous recovery method of triethylamine in VC production |
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| 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 |
Granted publication date: 20150708 Termination date: 20190127 |
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| CF01 | Termination of patent right due to non-payment of annual fee |