CN107099381A - Biodiesel prepares reaction unit - Google Patents

Abstract

The invention discloses a reaction device for preparing biodiesel, which comprises a reaction kettle. The reaction kettle is connected with an oil inlet pump and a raw oil storage tank through an oil inlet pipe; it is connected with a methanol pump and a methanol storage tank through a methanol feed pipe; The biodiesel storage tank is connected; it is connected with the condenser through the pipeline; it is connected with the waste liquid collection tank through the slag discharge pipe, and the slag discharge pipe is provided with a check valve and a valve; the oil inlet pipe and the methanol feed pipe are connected with the flow meter through the pipe , the valve and the check valve are connected; it also includes a methanol recovery tank and a rectification tower. The methanol recovery tank is connected to the condenser and the rectification tower through a pipeline; Pipe connection. Beneficial effects of the present invention: the amount of methanol passed into the reaction kettle per unit time is small, the time for esterification can be shortened and the moisture in the reactant can be quickly removed, the solid acid catalyst in the reaction kettle can be reused, and the methanol that has not participated in the reaction passes through The recovery and purification device can be reused.

Description

Biodiesel Preparation Reactor

technical field

The invention relates to the technical field of biodiesel preparation equipment, in particular to a reaction device for preparing biodiesel.

Background technique

As a clean and cheap renewable energy, biodiesel has developed rapidly in our country. The domestic large-scale biodiesel preparation process is based on the acid-base catalysis-based transesterification method. Most of the raw materials for biodiesel production are waste oils (gutter oil, hogwash oil, acidified oil, etc.), and the acid-base two-step method is generally used for production. Since the acid value of waste oil is generally high, usually greater than 100mgKOH/g, it needs to undergo acid-reducing pre-esterification treatment during alkali catalysis. This method generally uses methanol to react with free fatty acids and triglycerides in waste oils and fats to generate fatty acid methyl esters (biodiesel) under the catalytic action of a catalyst. During this process, excess methanol will be added to participate in the acid-reducing pre-esterification reaction. At the same time, in order to reduce production costs, excess methanol generally needs to be recovered by various methods; Catalyst loss. Because the existing deesterification reaction device generally has the disadvantages of high equipment cost, high anti-corrosion requirements, large amount of methanol consumption, low utilization rate, and long time for deesterification.

So the prior art needs to be improved and developed.

Contents of the invention

In view of the above, the present invention provides a reaction with high efficiency, simple operation, small amount of methanol consumption and high utilization rate, rapid removal of reaction water, shortening of acid reduction pre-esterification time, repeated use of solid acid catalyst and recovery of methanol device.

Technical solution of the present invention is:

A reaction device for preparing biodiesel, comprising a reactor 20 and a raw oil storage tank 36, a methanol storage tank 34, a crude biodiesel storage tank 38, a waste liquid collection tank 42, a condenser 14, and a reactor 20 respectively communicated with the reactor The outer wall is covered with a reactor jacket 19; the raw oil storage tank 36 is connected to the oil inlet pump 35 and the reactor 20 through the oil inlet pipe, the methanol storage tank 34 is connected to the methanol pump 35 and the reactor 20 through the methanol feed pipe 33, and the crude biodiesel storage tank 38 is communicated with the oil outlet branch pipe 27 in the reactor through the oil outlet pipe 25, the condenser 14 is communicated with the top of the reactor 20 through the outlet pipe 5, and the waste liquid collection tank 42 is communicated with the slag discharge pipe 28 of the reactor through a pipeline;

Also comprise methanol recovery tank 43, rectification tower 44 and vacuum pump 40, methanol recovery tank 43 is communicated with condenser 14 and rectification tower 44 by pipeline 60, rectification tower 44 is communicated with methanol storage tank 34 by methanol return pipe 46, vacuum pump 40 communicates with the waste liquid collection tank 42, the methanol recovery tank 43, and the crude biodiesel storage tank 38 through the pipeline 61; the condenser water inlet pipe 13 and the condenser water outlet pipe 16 communicate with the external cooling water pipe; It communicates with the external heating pipe through the pipeline, and the rectifying tower 44 communicates with the external pipeline through the condensate pipe 45. The oil inlet pipe 8 and the methanol feed pipe 33 are all provided with flow meters, valves and check valves, and the slag discharge pipe 28 is provided with The check valve 58 and the valve 59 communicate with the reaction kettle 20 .

The upper cover of the reaction kettle 20 is provided with a stirring motor 1 connected to two paddles 50 inside the reaction kettle 20 through the stirring shaft 21 .

The upper part of the reaction kettle 20 is provided with an inspection port 6, an exhaust pipe 3 with a valve, a pressure gauge 4 and a motor frame 2, and the inspection port 6, an exhaust pipe 3 with a valve and a pressure gauge 4 are all arranged on the top of the reaction kettle 20. Cover, motor frame 2 is arranged on the top of reaction kettle 20, is used for supporting stirring motor 1.

The upper part of the reaction kettle 20 is provided with a flushing pipe 18, and the flushing pipe 18 is fixed to the bracket 15 on the inner wall of the reaction kettle 20 with a pipe clamp, and communicated with the methanol pump 32 through an external pipeline.

A liquid level gauge 17 , a sampling tube 10 , a temperature probe 11 and an insulation layer 9 are provided on the outer wall of the middle part of the reaction kettle 20 . The liquid level 17 meter can conveniently observe the increase and decrease of the material in the reactor 20; the acid value of the raw material oil in the reactor 20 can be analyzed through the sampling monitoring of the sampling pipe 10; the insulation layer 9 can keep the jacket 19 of the reactor at a certain temperature, Reduce heat loss.

The lower part of the reaction kettle 20 is provided with a methanol branch pipe 23, and the methanol branch pipe 23 is fixed with a bracket on the inner wall of the reaction kettle and communicated with the methanol pipe 22, 24 and the methanol pump 32; the lower part of the reaction kettle 20 is provided with a slag discharge pipe 28. The pressure of the material in the kettle can discharge the material in the kettle to the waste liquid collection tank 42 through the slag discharge pipe 28 .

Each nozzle of the oil outlet branch pipe 27 is provided with a layer of 200-300 mesh copper mesh, and the copper mesh layer 49 and the oil outlet branch pipe 27 are fixed with pipe collars.

The external oil outlet pipe 25 of the reaction kettle 20 is provided with an inlet pipe 26 with a valve 63, and when the inlet pipe 26 communicates with the air outlet pipe of the compressor, it can wash out fine impurities on the copper mesh on the oil branch pipe 27.

The lower part of the methanol storage tank 34 communicates with the lower part of the rectification tower 44 through a pipeline.

The slag discharge pipe 28 can regularly discharge small impurities in the pipe to prevent the copper mesh layer 49 of the nozzle from clogging.

Beneficial effects of the present invention:

With the above structure, the amount of methanol introduced into the reaction kettle per unit time is small, which can shorten the acid-reducing pre-esterification time and quickly remove the moisture in the reactants, and can reuse the solid acid catalyst in the reaction kettle for many times. The reacted methanol can be reused through the recovery and purification device, which is conducive to promoting the development of biodiesel industrialization.

Description of drawings

Fig. 1 is a schematic diagram of the overall structure of the biodiesel preparation reaction device of the present invention.

Fig. 2 is a schematic diagram of the copper grid installation of the biodiesel preparation reaction device of the present invention.

Fig. 3 is a schematic diagram of the flushing pipe of the biodiesel preparation reaction device of the present invention.

Fig. 4 is a front view of the methanol branch pipe of the biodiesel preparation reaction device of the present invention.

Fig. 5 is a side view of the methanol branch pipe of the biodiesel preparation reaction device of the present invention.

Explanation of reference signs: 1—stirring motor; 2—motor bracket; 3—exhaust pipe; 4—pressure gauge; 5—air outlet pipe; 6—inspection port; 7—bolt; 8—oil inlet pipe; 10—sampling tube; 11—temperature probe; 12—heat conduction oil pipe; 13—inlet pipe of condenser; 14—condenser; 15—bracket; 16—water outlet pipe of condenser; 17—liquid level gauge; ― Reactor Jacket; 20 ― Reactor; 21 ― Stirring Shaft; 22 ― Methanol Pipe; 23 ― Methanol Branch Pipe; 24 ― Methanol Pipe; 25 ― Oil Outlet Pipe; Slag pipe; 29—reactor support; 30—valve; 31—flow meter; 32—methanol pump; 33—methanol feed pipe; 34—methanol storage tank; 35—inlet pump; 36—raw oil storage tank; 37— Empty pipe; 38—crude biodiesel storage tank; 39—pressure gauge; 40—vacuum pump; 41—liquid level gauge; 42—waste liquid collection tank; 43—methanol recovery tank; 44—distillation tower; 45—condensate pipe ; 46—methanol return pipe; 47—chemical pump; 48—drain pipe; 49—copper mesh layer; 50—blade; 51—check valve; 52—valve; 53—flow meter; Check valve; 56—condenser inlet; 57—condenser liquid outlet; 58—check valve; 59—valve; 60—pipeline; 61—pipeline; 62—pipeline.

detailed description

Example 1:

Referring to Fig. 1, a kind of biodiesel preparation reaction device comprises reactor 20, and reactor 20 is fixed on the reactor support 29, and reactor 20 and methanol storage tank 34, raw oil storage tank 36, crude biodiesel storage tank 38, The waste liquid collection tank 42, the methanol recovery tank 43, and the rectifying tower 44 are connected; the raw oil storage tank 36 is connected to the oil inlet pump 35 and the reaction kettle 20 through the oil inlet pipe 8, and the raw material oil storage tank 36 is provided with an emptying pipe 37, which can be used at different times. Raw material oil is emptied during use; Methanol storage tank 34 is communicated with methanol pump 32 and reactor 20 through methanol feed pipe 33; The biodiesel storage tank 38 is connected with a chemical pump 47, and the crude biodiesel in the crude biodiesel storage tank 38 can be pumped out to an external storage tank; the methanol recovery tank 43 is communicated with the condenser 14 and the rectification tower 44 through pipelines; the waste liquid The collection tank 42 is communicated with the slag discharge pipe 28 at the bottom of the reaction kettle through a pipeline; the rectification tower 44 is communicated with the methanol storage tank 34 through a methanol return pipe 46, and condensation water pipes 45 are arranged on both sides of the rectification tower 44 for dissolving the gaseous methanol Condensed into a liquid state, a pressure gauge 39 is also provided on the pipeline connected to the rectification tower to detect the pressure value in the rectification tower 44 .

The condenser 14 is communicated with the upper part of the reactor 20 through a pipeline, and the condenser water inlet pipe 13 and the condenser outlet pipe 16 are communicated with an external cooling water pipe; the inlet and outlet of the reactor jacket 19 are communicated with an external heating pipe through a pipeline; the rectification tower 44 communicates with external pipelines through condensate pipe 45; oil inlet pipe 8 and methanol feed pipe 33 are provided with flowmeter 31, valve 30 and check valve 51; slag discharge pipe 28 is provided with check valve 58 and valve 59 for reaction Kettle 20 is connected.

As shown in Fig. 2, Fig. 3 and Fig. 4, the lower part of the reaction kettle is provided with a methanol branch pipe 23, and the methanol branch pipe 23 is fixed with a bracket on the inner wall of the reaction kettle 20 and is communicated with the methanol pipe 22, 24 and the methanol pump 32; The bottom of the still 20 is provided with a slag discharge pipe 28, and a valve 63 is arranged on the slag discharge pipe 28. By utilizing the pressure of the material in the still, the material in the still can be discharged to the waste liquid collection tank 42 through the slag discharge pipe 28; the methanol branch pipe 23, outlet Each nozzle of the oil branch pipe 27 is provided with a layer of 200-300 mesh copper mesh layer 49, and the copper mesh layer 49 and the oil outlet branch pipe 27 are fixed with pipe hoops; the external oil outlet pipe 25 of the reactor 20 is provided with an air inlet pipe 26 with a valve When the inlet pipe 26 is communicated with the compressor air outlet pipe, the small impurities of the copper mesh layer 49 on the oil branch pipe 27 can be washed out.

Reactor 20 loam cake is connected with the sidewall of reactor 20 by bolt 7, and loam cake is also provided with inspection port 6, under the situation that reactor goes wrong, can only need to open inspection port 6 and can check and maintain. The upper cover of the reaction kettle 20 is also provided with a pressure gauge 4 for detecting the pressure value in the reaction kettle 20 . The side wall of the reaction kettle 20 is connected with a heat conduction oil pipe 12 for improving the heating capacity and uniformity and increasing the reaction speed. The side wall of the reaction kettle is also provided with a liquid level gauge 17, which is used to check the liquid capacity in the reaction kettle.

The outer wall of the reaction kettle is provided with a liquid level gauge 17, a sampling tube 10, a temperature probe 11, a reactor jacket 19 and an insulation layer 9; the liquid level gauge 17 can conveniently observe the increase or decrease of the material in the reactor 20; The monitoring can analyze the acid value of the raw material oil in the reactor 20; the insulation layer 9 can keep the jacket 19 of the reactor at a certain temperature and reduce heat loss.

The upper part of the reaction kettle 20 is provided with a flushing pipe 18, and the flushing pipe 18 is fixed with a bracket on the inner wall of the reaction kettle 20 with a pipe collar, and is communicated with a methanol pump 32 through an external pipeline.

A liquid level gauge 41 is also arranged on the outside of the waste liquid collection tank 42 for checking the increase or decrease of the liquid in the waste liquid collection tank 42 .

Concrete work process of the present invention is as follows:

The solid acid catalyst is added to the inside of the reaction kettle 20 through the exhaust pipe 3 according to the proportion of 5% of the mass of the raw material oil; the inlet and outlet valves of the jacket 19 of the reaction kettle are opened, and the heat source is introduced to heat up; The stirring motor 1 on the top and the cooling water are passed into the condenser 14, and the raw material oil in the raw oil storage tank 36 enters the inside of the reactor 20 through the oil inlet pipe 8, the valve 30, the flow meter 31 and the oil inlet pump 35; at the same time, the methanol storage tank 34 methanol through methanol pump 32, methanol pipe 24, flow meter 31, valve 30, methanol branch pipe 23 into the lower part of the reactor 20. The stirring shaft 21 drives the paddle 50 to rotate at the set stirring speed, and the raw material oil, solid acid catalyst and methanol undergo esterification reaction in the reaction kettle 20, and the methanol flows through the methanol pipe 24 through the set flow rate of the methanol pump 32. And the methanol branch pipe 23 enters the lower part of the reaction kettle 20. During the reaction process, the excess methanol gas, the original moisture of the raw material oil and the water vapor generated by the reaction enter into the reaction kettle 20 through the gas outlet 56 of the upper part of the reaction kettle 20. The condenser 14, after being cooled by cooling water, becomes liquid and flows into the methanol recovery tank 43 through the liquid outlet 57 through the pipeline 60; the methanol gas formed under the high-temperature heating of the raw material oil enters the reaction kettle 20 through each methanol branch pipe 23 to be mixed with the raw material oil and Catalyst reaction: the crude biodiesel produced after the reaction flows into the crude biodiesel storage tank 38 through the oil outlet pipe branch pipe 27 and the oil outlet pipe 25, and the solid acid catalyst of the reactor 20 can continue to flow in the reactor 20 under the copper mesh layer 49 blocking First use; the remaining waste liquid in the reactor 20 flows into the waste liquid collection tank 42 through the slag discharge pipe 28. The insulation layer 9 of the outer wall of the reactor jacket 19 can keep a certain temperature in the jacket, and the acid reduction and pre-esterification of the raw material oil in the reactor 20 can be regularly analyzed by sampling through the sampling tube 10; The internal negative pressure can accelerate the methanol gas and water vapor in the reactor 20 to enter the methanol recovery tank 43, and can also accelerate the crude biodiesel in the reactor 20 to flow into the storage tank.

In Example 1, the process of preparing biodiesel by acid reduction pre-esterification of 5 tons of waste oil with an acid value of 120 mgKOH/g was taken as an example. inside of the reactor 20; open the inlet and outlet valves of the jacket 19 of the reaction kettle, feed the heat source to heat up; at the same time, turn on the stirring motor 1 and feed the cooling water into the condenser 14, and the raw oil in the raw oil storage tank 36 passes through the oil inlet pipe 8. The valve 30, the flow meter 31 and the oil inlet pump 35 enter the reactor 20; at the same time, the methanol in the methanol storage tank 34 enters the reactor 20 through the methanol pump 32, the methanol pipe 24, the flow meter 31, the valve 30, and the methanol branch pipe 23 lower part. Raw material oil, solid acid catalyst and methanol are carried out in the reaction kettle 20 with a stirring speed of 150rpm/min to carry out the esterification reaction, and the methanol with the flow rate set by the methanol pump 32 enters the reaction kettle 20 through the methanol pipe 24 and the methanol branch pipe 23 The lower part, during the reaction process, the excess methanol gas, the original moisture of the raw material oil and the water vapor generated by the reaction at high temperature enter the condenser 14 from the gas outlet 56 in the upper part of the reactor 20, and form a liquid after cooling Flow into the methanol recovery tank 43 from the liquid outlet 57 through the pipeline 60; the methanol gas formed under the high-temperature heating of the raw material oil enters the reaction kettle 20 through each methanol branch pipe 23 to react with the raw material oil and the catalyst; the crude biodiesel produced after the reaction passes through the outlet The oil pipe branch pipe 27 and the oil outlet pipe 25 flow into the crude biodiesel storage tank 38, and the solid acid catalyst in the reactor 20 can continue to be used in the reactor for many times under the obstruction of the copper mesh layer 49; the remaining waste liquid in the reactor passes through the slag discharge pipe 28 flows into the waste liquid collection tank 42. The insulation layer 9 of the outer wall of the reactor jacket 19 can keep a certain temperature in the jacket, and the acid reduction and pre-esterification of the raw material oil in the reactor can be regularly analyzed by sampling through the sampling tube 10; Negative pressure can accelerate the methanol gas and water vapor in the reactor to enter the methanol recovery tank 43, and can also accelerate the crude biodiesel in the reactor to flow into the storage tank. Open the valve on the exhaust pipe 3 to replenish the new solid acid catalyst to the reactor 20 regularly. After opening the valve 54 and the methanol pump 32 through the flushing pipe 18 in the upper part of the reaction kettle, methanol can be pumped into the inner wall of the reaction kettle 20, and the flushing waste liquid is discharged to the waste liquid collection tank 42 through the slag discharge pipe 28. Using this device can shorten the acid-reducing pre-esterification time and quickly remove the water in the reactant, and can reuse the solid acid catalyst in the reaction kettle for many times, and the methanol that has not participated in the reaction can be reused through the recovery and purification device.

The above detailed description is a specific description of the feasible embodiment of the present invention. This embodiment is not used to limit the patent scope of the present invention. Any equivalent implementation or change that does not deviate from the present invention should be included in the patent scope of this case. middle.

Claims (10)

1. a kind of biodiesel prepares reaction unit, it is characterised in that：Including

Rabbling mechanism is provided with inside reactor (20), the reactor (20), pressure gauge (4) is above covered with, side wall is provided with temperature Pop one's head in (11), and outer wall is arranged with reacting kettle jacketing (19), the import and export of the reacting kettle jacketing (19) passes through heat-conducting oil pipes And ft connection (12)；

Raw material oil tank (36), an oil-feed pump (35), the other end connection institute of the oil-feed pump (35) are connected by oil inlet pipe (8) Reactor (20) is stated, the oil inlet pipe (8) is provided with flowmeter (53), valve (54) and check-valves (55)；

Methanol tank (34), methanol pump (32) is connected by methanol feed pipe (33), and the other end of the methanol pump (32) passes through Methanol feed pipe (33) connects the methanol pipe (24) of reactor (20) bottom, and the methanol feed pipe (33) is provided with flow Count (31), valve (30) and check-valves (51)；

Coarse biodiesel storage tank (38), the bottom of the reactor (20) is connected by flowline (25)；

Waste collection tank (42), the reactor (20) is connected by scum pipe (28), and the scum pipe (28) is provided with non-return Valve (58) and valve (59), the scum pipe (28) connect with the bottom of reactor (20)；

Condenser (14), is arranged at the outer wall of the reactor (20), and the condenser air inlet (56) is connected by escape pipe (5) Lead to the top of the reactor (20), water inlet pipe (13), the outlet pipe (16) of the condenser (14) connect with outside cooling water pipe It is logical；

Methanol Recovery tank (43), is interconnected by pipeline (60) and the condenser liquid outlet (57) and a rectifying column (44), Rectifying column (44) bottom connects the Methanol Recovery tank (43), and top connects the methanol by methanol eddy pipe (46) and stored up Tank (34).

2. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：Also include vavuum pump (40), institute State vavuum pump (40) and pass through pipeline (61) and the waste collection tank (42), the Methanol Recovery tank (43) and the coarse biometric bavin Oil tank (38) is connected.

3. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：The rabbling mechanism includes setting In the electric motor stand (2) covered on reactor, and the stirring motor (1) being fixed on the electric motor stand (2), the stirring motor (1) agitating shaft (21) is connected through lid is vertical with the blade (50) inside reactor on the reactor (20), the blade (50) it is anchor formula stirrer paddle.

4. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：Reactor (20) upper surface Provided with access hole (6).

5. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：Reactor (20) internal upper part Provided with flush pipe (18), the flush pipe (18) and the support of reactor (20) inwall are fixed, and flush pipe (18) passes through pipeline (62) connected with methanol pump (32).

6. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：The interior bottom of the reactor (20) Provided with methanol branch pipe (23), the methanol branch pipe (23) and the support of reactor inwall are fixed and by methanol pipe (24) and methanol Pump (32) is connected.

7. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：Reactor (20) bottom is set There is oil outlet branch pipe (27), the oil outlet branch pipe (27) is made up of two orthogonal and intercommunication pipelines, the oil outlet branch pipe (27) each mouth of pipe is installed with copper mesh layers (49) by pipe collar.

8. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：The mesh number of the copper mesh layers (49) For 200-300 mesh.

9. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：The flowline (25) is provided with Valve (63) is provided with air inlet pipe (26), the air inlet pipe (26).

10. biodiesel according to claim 1 prepares reaction unit, it is characterised in that：Reactor (20) outer wall Provided with heat-insulation layer (9), heat-insulation layer (9) can make reacting kettle jacketing (19) keep certain temperature, reduce the loss of heat.