CN201711153U - Experimental device for tetraethyl lead preparation with Grignard reagents - Google Patents
Experimental device for tetraethyl lead preparation with Grignard reagents Download PDFInfo
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- CN201711153U CN201711153U CN2010202483460U CN201020248346U CN201711153U CN 201711153 U CN201711153 U CN 201711153U CN 2010202483460 U CN2010202483460 U CN 2010202483460U CN 201020248346 U CN201020248346 U CN 201020248346U CN 201711153 U CN201711153 U CN 201711153U
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Abstract
The utility model discloses an experimental device for tetraethyl lead preparation with Grignard reagents, which comprises a four-neck flask, a thermostat water bath, an electric stirrer, a condenser, a constant pressure funnel and a nitrogen cylinder. The lower half part of the four-neck flask is arranged inside the thermostat water bath; a fluoroethylene stirring rod is connected with the electric stirrer and passes through a porcelain sleeve to be inserted into the four-neck flask; the condenser is arranged on a left support rack, one end of the condenser is inserted in the left opening of the four-neck flask, and the other end thereof is provided with a drying tube; and the constant pressure funnel is arranged on a right support rack, and the lower end of the constant pressure funnel is inserted in the middle opening of the four-neck flask. The nitrogen cylinder is connected with a nitrogen gas needle through a hose, and the nitrogen gas needle is inserted in the middle opening of the four-neck flask. The experimental device provided by the utility model has the advantages of simple and feasible structure, stable reaction, burst explosion resistance, high lead conversion rate, and high success ratio.
Description
Technical field
The utility model relates to the breadboard preparation facilities of a kind of lead tetraethide, for pilot plant provides design parameter, belongs to chemical industry, because alkyl lead toxicity is extremely strong, the utility model relates in particular to the experimental provision that a kind of green reagent legal system is equipped with lead tetraethide.
Background technology
The green reagent method is produced lead tetraethide [Pb (C
2H
5)
4] have advantages such as investing little, plumbous conversion ratio height, the easy control of safety than plumbous zinc sodium high pressure synthesis technique, but in preparation during green reagent, especially during dripping bromine ethane, occur quick-fried easily towards phenomenon, need obtain optimization control parameter by experiment, experimental provision is particularly important for this reason.
The utility model content
The technical problems to be solved in the utility model is: overcome the existing apparatus deficiency, a kind of simple, reacting balance be provided, prevent from quick-friedly to dash, plumbous conversion ratio height, experimental provision that success rate is high, for the important material reaction concentration of acquisition, temperature, hydrolysis rate, the technical conditions of solvent recovery, multinomial technical parameter are produced in batch production, thereby make the Process configuration of batch production more be tending towards reasonable, practical.
The technical scheme in the invention for solving the technical problem is: a kind of green reagent legal system is equipped with the experimental provision of lead tetraethide, by four-hole boiling flask, thermostat water bath, electric mixer, condenser, constant pressure funnel, nitrogen cylinder is formed, the latter half of described four-hole boiling flask is placed in thermostat water bath inside, bottle mouth position seals by porcelain bushing shell in the middle of the described four-hole boiling flask, be connected with the PVF stirring rod on the described electric mixer, described PVF stirring rod is passed porcelain bushing shell and is assigned into four-hole boiling flask inside, point for measuring temperature device in bottle mouth position has been assigned in the middle of the described four-hole boiling flask, described interior point for measuring temperature device passes porcelain bushing shell.
Described condenser is installed on the bracing frame of left side by test tube clamp, described condenser one end assigns into the left side bottle mouth position of four-hole boiling flask, described condenser bodies partly is provided with two cooling water interfaces, the described condenser other end is equipped with drying tube, drier is laid in described drying tube inside, and described drier is anhydrous calcium chloride and absorbent cotton wool.
Described constant pressure funnel is installed on the bracing frame of right side, and described constant pressure funnel lower end assigns into the bottle mouth position on four-hole boiling flask right side.
Outer point for measuring temperature device is laid in described thermostat water bath inside, and described outer point for measuring temperature device is installed on the bracing frame of right side by cross bar.
Described nitrogen cylinder is connected with the nitrogen syringe needle by flexible pipe, and described nitrogen syringe needle assigns into the middle bottle mouth position of four-hole boiling flask.
The utlity model has following remarkable advantages and beneficial effect:
1) operation is simple, reacting balance, prevent quick-fried dashing;
2) plumbous conversion ratio height, success rate height.
Description of drawings
Fig. 1 is equipped with the floor map of the experimental provision of lead tetraethide for a kind of green reagent legal system;
Wherein: the 1-four-hole boiling flask; The 2-thermostat water bath; The 3-electric mixer; 4-PVF stirring rod; The 5-constant pressure funnel; The 6-condenser; The 7-porcelain bushing shell; Point for measuring temperature device in the 8-; The outer point for measuring temperature device of 9-; 10-right side bracing frame; 11-left side bracing frame; The 12-drying tube; The 13-nitrogen cylinder; The 14-cross bar; The 15-test tube clamp; 16-cooling water interface; 17-nitrogen syringe needle.
The specific embodiment
As shown in Figure 1: a kind of green reagent legal system is equipped with the experimental provision of lead tetraethide, by four-hole boiling flask 1, thermostat water bath 2, electric mixer 3, condenser 6, constant pressure funnel 5, nitrogen cylinder 13 is formed, the latter half of four-hole boiling flask 1 is placed in thermostat water bath 2 inside, bottle mouth position is by porcelain bushing shell 7 sealings in the middle of the four-hole boiling flask 1, be connected with PVF stirring rod 4 on the electric mixer 3, PVF stirring rod 4 is passed porcelain bushing shell 7 and is assigned into four-hole boiling flask 1 inside, point for measuring temperature device 8 in bottle mouth position has been assigned in the middle of the four-hole boiling flask 1, be used to measure the four-hole boiling flask internal temperature, interior point for measuring temperature device 8 passes porcelain bushing shell 7; Condenser 6 is installed on the bracing frame 11 of left side by test tube clamp 15, condenser 6 one ends assign into the left side bottle mouth position of four-hole boiling flask 1, condenser 6 main parts are provided with two cooling water interfaces 16, condenser 6 other ends are equipped with drying tube 12, drier is laid in drying tube 12 inside, and drier is anhydrous calcium chloride and absorbent cotton wool; Constant pressure funnel 5 is installed on the right side bracing frame 10, and constant pressure funnel 5 lower ends assign into the bottle mouth position on four-hole boiling flask 1 right side; Outer point for measuring temperature device 9 is laid in thermostat water bath 2 inside, and outer point for measuring temperature device 9 is installed on the right side bracing frame 10 by cross bar 14, outer point for measuring temperature device 9 main thermostat water bath 2 temperature inside of measuring; Nitrogen cylinder 13 is connected with nitrogen syringe needle 17 by flexible pipe, and nitrogen syringe needle 17 assigns into the middle bottle mouth position of four-hole boiling flask 1.
The utility model is to implement like this: open the valve of nitrogen cylinder 13, clean four-hole boiling flask 1 with oxolane, install to put and prepare all parts, after solvents tetrahydrofurane (THF) and magnesium chips are poured into four-hole and burnt face 1 inside, add catalyst I again
2After, opening electric mixer 3 stirs, press funnel 5 dripping bromine ethane by weighing apparatus, the cooling water interface 16 of open cold condenser when four-hole boiling flask 1 first half inwall has dew point, note the temperature of point for measuring temperature device 8 in each elementary reaction and the variations in temperature relation of outer point for measuring temperature device 9 simultaneously, until reaction end, promptly accuse the green reagent preparation and finish.
It should be noted that at last: above embodiment only in order to the explanation the utility model and and the described technical scheme of unrestricted the utility model; Therefore, although this specification has been described in detail the utility model with reference to each above-mentioned embodiment,, those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the utility model; And all do not break away from the technical scheme and the improvement thereof of spirit and scope of the present utility model, and it all should be encompassed in the claim scope of the present utility model.
Claims (7)
1. a green reagent legal system is equipped with the experimental provision of lead tetraethide, form by four-hole boiling flask, thermostat water bath, electric mixer, condenser, constant pressure funnel, nitrogen cylinder, it is characterized in that: the latter half of described four-hole boiling flask is placed in thermostat water bath inside, bottle mouth position seals by porcelain bushing shell in the middle of the described four-hole boiling flask, point for measuring temperature device in bottle mouth position has been assigned in the middle of the described four-hole boiling flask, described interior point for measuring temperature device passes porcelain bushing shell.
2. a kind of green reagent legal system according to claim 1 is equipped with the experimental provision of lead tetraethide, it is characterized in that: be connected with the PVF stirring rod on the described electric mixer, described PVF stirring rod is passed porcelain bushing shell and is assigned into four-hole boiling flask inside.
3. a kind of green reagent legal system according to claim 1 is equipped with the experimental provision of lead tetraethide, it is characterized in that: described condenser is installed on the bracing frame of left side by test tube clamp, described condenser one end assigns into the left side bottle mouth position of four-hole boiling flask, described condenser bodies partly is provided with two cooling water interfaces, and the described condenser other end is equipped with drying tube.
4. a kind of green reagent legal system according to claim 3 is equipped with the experimental provision of lead tetraethide, it is characterized in that: drier is laid in described drying tube inside, and described drier is anhydrous calcium chloride and absorbent cotton wool.
5. a kind of green reagent legal system according to claim 1 is equipped with the experimental provision of lead tetraethide, it is characterized in that: described constant pressure funnel is installed on the bracing frame of right side, and described constant pressure funnel lower end assigns into the bottle mouth position on four-hole boiling flask right side.
6. a kind of green reagent legal system according to claim 1 is equipped with the experimental provision of lead tetraethide, it is characterized in that: outer point for measuring temperature device is laid in described thermostat water bath inside, and described outer point for measuring temperature device is installed on the bracing frame of right side by cross bar.
7. a kind of green reagent legal system according to claim 1 is equipped with the experimental provision of lead tetraethide, it is characterized in that: described nitrogen cylinder is connected with the nitrogen syringe needle by flexible pipe, and described nitrogen syringe needle assigns into the middle bottle mouth position of four-hole boiling flask.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202483460U CN201711153U (en) | 2010-07-06 | 2010-07-06 | Experimental device for tetraethyl lead preparation with Grignard reagents |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202483460U CN201711153U (en) | 2010-07-06 | 2010-07-06 | Experimental device for tetraethyl lead preparation with Grignard reagents |
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| Publication Number | Publication Date |
|---|---|
| CN201711153U true CN201711153U (en) | 2011-01-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010202483460U Expired - Fee Related CN201711153U (en) | 2010-07-06 | 2010-07-06 | Experimental device for tetraethyl lead preparation with Grignard reagents |
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| CN (1) | CN201711153U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102179224A (en) * | 2011-03-11 | 2011-09-14 | 吕元 | Solar reaction kettle |
| CN104004014A (en) * | 2014-04-17 | 2014-08-27 | 孙宝生 | Preparation method for tetraethyllead fuel oil antiknock additive and fuel oil antiknock additive |
| CN106422985A (en) * | 2016-11-30 | 2017-02-22 | 南京睿宇物联网科技有限公司 | Reaction system for safely adding tert-butyllithium into reactor |
-
2010
- 2010-07-06 CN CN2010202483460U patent/CN201711153U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102179224A (en) * | 2011-03-11 | 2011-09-14 | 吕元 | Solar reaction kettle |
| CN104004014A (en) * | 2014-04-17 | 2014-08-27 | 孙宝生 | Preparation method for tetraethyllead fuel oil antiknock additive and fuel oil antiknock additive |
| CN106422985A (en) * | 2016-11-30 | 2017-02-22 | 南京睿宇物联网科技有限公司 | Reaction system for safely adding tert-butyllithium into reactor |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110119 Termination date: 20130706 |