Efficient recovery system for high-boiling residues in organic silicon pulp residues

Abstract

The utility model discloses a high-efficiency recovery system for high-boiling residues in organic silicon pulp residues, which comprises a filter press and a phase separator, an intermediate separator is arranged between the filter press and the phase separator, the intermediate separator comprises an intermediate separation tank and a cyclone separation tank, an inner separation cylinder with a sealed top is mounted at the upper part in the intermediate separation tank in a penetrating manner, and the cyclone separation tank is arranged in the middle separation tank. A filter screen is installed on the lower portion in the inner separation cylinder, a spiral slag extractor is installed on the upper side of the filter screen, a slag storage tank is connected to a slag discharge port of the filter press and a slag discharge port of the spiral slag extractor, a liquid guide port of the cyclone separation tank is communicated with the filter press, a top outlet of the cyclone separation tank is communicated with the phase separator, a high-boiling-point substance outlet of the phase separator is connected with a high-boiling-point substance storage tank, and the high-boiling-point substance storage tank is connected with a high-boiling-point substance outlet of the phase separator. Acid liquor outlets of the intermediate separation tank and the phase separator are connected with a hydrochloric acid storage tank. The device not only is favorable for reducing the impurity rate of the separated high-boiling-point substance, but also can realize thorough separation of the high-boiling-point substance and diluted hydrochloric acid, and realizes efficient recovery of the high-boiling-point substance.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the organic silicon production processing technical field, concretely relates to a kind of efficient recovery system of high-boiling substance in organic silicon slurry residue. BACKGROUND

[0002] The synthesis of organic silicon monomer mainly adopts direct method, that is, methyl chloride and industrial silicon are reacted in fluidized bed in fluidized state under the action of copper-based catalyst to obtain crude monomer mainly composed of dimethyldichlorosilane ((CH3)2SiCl2). In the above reaction process of methyl chloride and industrial silicon, high-boiling byproduct of methyl chlorosilane is used to wet dust the synthesized methyl chlorosilane mixture, generating a paste-like liquid-solid mixture with a color of soy sauce. This mixture is simply referred to as organic silicon slurry residue. The main components of organic silicon slurry residue are more high-boiling substance and a small amount of silicon powder (particle size of 2-150 um) brought out by fluidized bed, copper powder and trace elements Fe, Zn, Al, Sn, etc. The high-boiling substance with a boiling range of 70.5-250 ℃ is mainly composed of disilane, siloxane and methyl chloride, and the solid content is 20-25%. Organic silicon slurry residue is flammable and volatile, and can easily cause strong acid mist and combustion if exposed to air. Therefore, it must be treated in a harmless manner. At present, the treatment of organic silicon slurry residue is mostly carried out by hydrolysis method. The hydrolysis method for disposing organic silicon slurry residue is to first hydrolyze the organic silicon slurry residue with dilute hydrochloric acid, and then separate the high-boiling substance by pressure filtration. In the existing technology, the recovery of high-boiling substance from organic silicon slurry residue is first carried out by pressure filtration of the hydrolyzed organic silicon slurry residue, then the slurry obtained by pressure filtration is separated by a phase separator to obtain high-boiling substance. The above high-boiling substance recovery device has the following disadvantages in use: first, the slurry after pressure filtration still contains slurry residue with a relatively small particle size. The slurry after pressure filtration is directly separated in the phase separator, and the slurry content in the separated high-boiling substance is large, which affects the quality of high-boiling substance; second, the slurry is directly separated in the phase separator by relying on the principle of different densities, which cannot achieve complete separation of high-boiling substance, and the separation effect is not ideal, and the recovery rate of high-boiling substance is low. Therefore, it is an urgent need to develop an efficient recovery system for high-boiling substance in organic silicon slurry residue, which has reasonable structure, low impurity content and remarkable separation effect of high-boiling substance. SUMMARY

[0003] The utility model aims at providing an efficient recovery system for high-boiling substance in organic silicon slurry residue, which has reasonable structure, low impurity content and remarkable separation effect of high-boiling substance.

[0004] The utility model discloses a purpose is realized like this, including filter press and phase separator, be provided with intermediate separator between filter press and phase separator, and intermediate separator includes intermediate separation jar and cyclone separation jar, and the upper portion of inside separation cylinder is installed to the top seal in the intermediate separation jar, and the lower portion of inside separation cylinder is installed with filter screen, and the inside separation cylinder on filter screen upper side installs the spiral deslagging machine extending to the outside of intermediate separation jar, and the deslagging mouth of filter press and spiral deslagging machine all are connected with the residue storage groove through the residue pipe, and the cyclone separation jar is installed in the upper portion of inside separation cylinder and communicates with it, and the inner wall of cyclone separation jar is provided with the cyclone groove of helical structure, and the upper portion tangential installation of cyclone separation jar has the liquid guide, and the liquid guide communicates with the liquid outlet of filter press through the first communication pipe, and the top outlet of cyclone separation jar communicates with the liquid inlet of phase separator through the second communication pipe, and the high boiling point material outlet of phase separator is connected with high boiling point material storage jar, and the acid liquid outlet of intermediate separation jar and phase separator all are connected with the hydrochloric acid storage jar through the acid discharge pipe.

[0005] Compared with the prior art, the device has the advantages that: the device is provided with a cyclone separation jar and an intermediate separation jar between the filter press and the phase separator, the cyclone separation jar utilizes the principle of centrifugal separation to make the slurry in a spiral motion state in the cyclone separation jar, the high boiling point material and the dilute hydrochloric acid have different densities, and after centrifugal separation, the slurry can be pre-separated, the cyclone separation jar can reduce the separation burden of the subsequent phase separator, and is conducive to improving the separation effect of the subsequent high boiling point material, the intermediate separation jar can filter the separated slurry again, avoid too many impurities from entering the phase separator to affect the quality of the high boiling point material, which is conducive to reducing the impurity content of the high boiling point material after separation and the slurry residue in the slurry, which can reduce the impurity content of the slurry entering the phase separator, improve the product quality of the high boiling point material, and after the pre-separated and filtered slurry enters the phase separator, the high boiling point material and the dilute hydrochloric acid can be completely separated, thereby realizing efficient recovery of the high boiling point material, the device has the advantages of reasonable structure, convenient use, good solid-liquid separation effect, high high boiling point material recovery rate, and easy popularization and use. BRIEF DESCRIPTION OF DRAWINGS

[0006] Fig. 1 It is the whole structure schematic diagram of the utility model;

[0007] Fig. 2 It is the structure schematic diagram of filter press 1 in the utility model;

[0008] In the figure: 1 - filter press, 101 - outer shell, 102 - filter press cylinder, 103 - sealing plate, 104 - feeding pipe, 105 - spiral extrusion shaft, 106 - feeding rotating shaft, 107 - driving motor, 108 - discharging rotating shaft, 109 - slag receiving hopper, 110 - liquid leakage hole, 2 - phase separator, 3 - intermediate separation tank, 301 - inner separation cylinder, 302 - filter screen, 303 - spiral slag discharging machine, 304 - overflow port, 305 - overflow tank body, 306 - bypass pipe, 307 - baffle, 4 - cyclone separation tank, 401 - liquid guide port, 5 - slag discharging pipe, 6 - slag storage groove, 7 - first communication pipe, 8 - second communication pipe, 9 - high-boiling substance storage tank, 10 - acid discharging pipe, 11 - hydrochloric acid storage tank. DETAILED DESCRIPTION

[0009] The utility model makes further explanation in connection with the drawings, but not in any way to the utility model add restrictions, based on the utility model teach to make any change or improvement, all belong to the protection scope of the utility model.

[0010] As Figs. 1-2 shown, the utility model, including filter press 1 and phase separator 2, phase separator 2 adopts two-phase separator used in prior art, be provided with intermediate separator between filter press 1 and phase separator 2, the intermediate separator includes intermediate separation tank 3 and cyclone separation tank 4, the upper portion of the inner separation cylinder 301 of the upper portion of the intermediate separation tank 3 is installed through the top sealing, the lower portion of the inner separation cylinder 301 is installed with filter screen 302, and the inner separation cylinder 301 on the upper side of filter screen 302 is installed with spiral slag discharging machine 303 extending to the outside of intermediate separation tank 3, and the spiral slag discharging machine 303 includes slag discharging pipe, spiral shaft and motor and other components, the motor drives the spiral shaft to rotate, and the spiral shaft can timely discharge the slag gathered on the filter screen from the inner separation cylinder in the process of rotating, the slag discharging port of filter press 1 and spiral slag discharging machine 303 is connected with the slag storage groove 6 through slag discharging pipe 5, the cyclone separation tank 4 is installed above the inner separation cylinder 301 and communicates with it, the inner wall of the cyclone separation tank 4 is provided with cyclone groove of spiral structure, the tangential installation of the upper portion of the cyclone separation tank 4 is provided with liquid guide port 401, the liquid guide port 401 communicates with the liquid outlet of filter press 1 through the first communication pipe 7, the top outlet of the cyclone separation tank 4 communicates with the liquid inlet of phase separator 2 through the second communication pipe 8, the high-boiling substance outlet of phase separator 2 is connected with high-boiling substance storage tank 9, and the acid liquid outlet of intermediate separation tank 3 and phase separator 2 is connected with hydrochloric acid storage tank 11 through acid discharging pipe 10.

[0011] The working process of the system is: after hydrochloric acid hydrolysis, the organic silicon slurry residue enters the filter press 1 for solid-liquid separation, the slurry residue separated out by solid-liquid separation enters the slurry storage tank 6 through the slurry discharge pipe 5, the slurry separated out by solid-liquid separation enters the cyclone separation tank 4 tangentially from the liquid guide port 104 through the first communication pipe 7, the cyclone separation tank 4 is processed with a spiral cyclone groove, the slurry enters the cyclone separation tank 4 and is subjected to the action of centrifugal force, the slurry can be in a spiral motion state in the cyclone separation tank 4, and since the densities of the high-boiling substance and the dilute hydrochloric acid are different, the slurry can be pre-separated to separate the dilute hydrochloric acid and the high-boiling substance in the slurry, the slurry separated by centrifugation falls into the inner separation cylinder 301, and after being filtered and intercepted by the filter screen 302, the slurry can be filtered, the slurry residue filtered and intercepted is discharged from the intermediate separation tank 3 by the spiral slurry discharge machine 303 and then enters the slurry storage tank 6, the slurry containing dilute hydrochloric acid separated by centrifugation flows out from the inner separation cylinder 302 and enters the intermediate separation tank 3, and after being separated again, it enters the hydrochloric acid storage tank 11 from the acid discharge pipe 10, and the slurry containing high-boiling substance separated by centrifugation overflows from the top outlet of the centrifugal separation tank 4, and then enters the phase separator 9 through the second communication pipe 8 for further phase separation, the slurry containing high-boiling substance is separated by phase separation, and according to the principle of different densities, the high-boiling substance and the dilute hydrochloric acid can be completely separated, the high-boiling substance separated by phase separation is discharged from the high-boiling substance outlet and stored in the high-boiling substance storage tank 9, and the dilute hydrochloric acid separated by phase separation enters the hydrochloric acid storage tank 11 through the acid discharge pipe 10, and the dilute hydrochloric acid in the hydrochloric acid storage tank 11 can be returned to the hydrolysis system for recycling, the system uses the filter press 1, the intermediate separator and the phase separator 2 in cooperation, can realize efficient recovery of high-boiling substance, has the advantages of reasonable structure, convenient use, good solid-liquid separation effect, and high high-boiling substance recovery rate.

[0012] The filter press can use the plate and frame filter press in the prior art. In order to improve the production efficiency, the filter press 1 comprises an outer shell 101 and a filter cylinder 102 fixedly installed in the outer shell 101, a sealing plate 103 is installed at the feeding end of the filter cylinder 102, the discharging end of the filter cylinder 102 is in an open structure, a feeding pipe 104 extending above the outer shell is arranged at the top of the filter cylinder 102 close to the sealing plate 103, a spiral extrusion shaft 105 is coaxially installed in the filter cylinder 102, a feeding rotating shaft 106 is installed at one end of the spiral extrusion shaft 105, the feeding rotating shaft 106 is rotatably installed at one end of the outer shell 101 after penetrating through the sealing plate 103, a driving motor 107 is installed on the outer shell 101 and is in driving connection with the feeding rotating shaft 106, the driving motor 107 is a structure used in the prior art, and a finished product can be directly purchased according to the power used, a discharging rotating shaft 108 is installed at the other end of the spiral extrusion shaft 105, the discharging rotating shaft 108 is rotatably installed at the other end of the outer shell 101, a slag receiving hopper 109 is installed on the outer shell 101 below the discharging end of the filter cylinder 102, the slag discharge port is arranged at the bottom of the slag receiving hopper 109, a plurality of liquid leakage holes 110 are arranged at the bottom of the filter cylinder 102, and a liquid outlet is arranged at the bottom of the outer shell 101. After the hydrolyzed organic silicon slurry is subjected to the filter pressing treatment, the organic silicon slurry enters the filter cylinder 102 from the feeding pipe 104, then the driving motor 107 is started, the driving motor 107 drives the spiral extrusion shaft 105 and the discharging rotating shaft 108 to rotate through the feeding rotating shaft 106, the spiral extrusion shaft 105 can extrude the organic silicon slurry in the process of rotating, so that the slurry liquid in the organic silicon slurry falls to the bottom of the outer shell 101 through the liquid leakage holes 110 and is finally discharged through the liquid outlet, and the slurry in the organic silicon slurry falls into the slag receiving hopper 109 from the discharging end of the filter cylinder 102 after being spirally conveyed by the spiral extrusion shaft 105 and is finally discharged through the slag discharge port. After the driving motor 107 is started, the organic silicon slurry can be continuously added from the feeding pipe 104, the organic silicon slurry can be quickly subjected to the solid-liquid separation, and the efficiency of the solid-liquid separation is improved.

[0013] In order to timely discharge the slurry liquid at the bottom of the outer shell 101 from the outer shell 101, the bottom of the outer shell 101 is arranged in a structure that the middle part is low and the two ends are high, and the liquid outlet is arranged at the middle part of the outer shell 101. The slurry liquid falling into the outer shell 101 flows from the two ends to the middle part of the outer shell 101, so that the liquid discharging speed is improved.

[0014] In order to improve the filtering effect of the filter cylinder 102 and greatly reduce the impurity content of the slurry liquid, a gauze is arranged in the liquid leakage hole 110. The gauze can be arranged in a multi-layer structure according to the use requirement.

[0015] In order to improve the effect of solid-liquid separation, the diameter of the screw extrusion shaft 105 gradually increases from the feed end to the discharge end, and the filter space in the filter cylinder 102 gradually decreases from the feed end to the discharge end, so that the screw extrusion shaft 105 can fully contact with the silicone slurry residue, and the extrusion of the screw extrusion shaft 105 can improve the effect of solid-liquid separation.

[0016] Further, in order to facilitate the slurry residue accumulated on the filter screen 302 to be discharged from the inner separation cylinder 301 in time, the filter screen 302 is arranged inclined in the inner separation cylinder 301, and the screw residue discharger 303 is arranged in cooperation with the filter screen 302, and the residue discharge port of the screw residue discharger 303 is arranged at one side of the lower end of the filter screen 302.

[0017] In order to realize efficient recovery of high-boiling substances, the upper part of the intermediate separation tank 3 is provided with an overflow port 304, and an overflow tank body 305 is sealingly installed outside the intermediate separation tank 3 outside the overflow port 304, and the bottom of the overflow tank body 305 is provided with a bypass pipe 306 communicated with the second communication pipe 8. The high-boiling substances may still be contained in the dilute hydrochloric acid separated out by the inner separation cylinder 301, and according to the different densities, the high-boiling substances separated out in the intermediate separation tank 3 are accumulated on the surface of the dilute hydrochloric acid. With the gradual rising of the liquid level in the intermediate separation tank 3, the separated high-boiling substances will enter the overflow tank body 305 through the overflow port 304, and then enter the phase separator 4 through the bypass pipe 306, so as to realize efficient recovery of high-boiling substances.

[0018] Further, in order to slow down the flow speed of the silicone slurry in the inner separation cylinder 301, a plurality of baffles 307 are installed staggered up and down in the inner separation cylinder 301 above the screw residue discharger 303, and the baffles 307 are arranged inclined downward in the inner separation cylinder 301. The arrangement of the baffles 307 can slow down the flow speed of the silicone slurry in the inner separation cylinder 301, so as to improve the filtering effect of the filter screen 302 and further improve the separation effect of the cyclone separation tank 4.

Claims

1. An efficient recovery system for high-boiling substances in organosilicon slurry, comprising a filter press (1) and a phase separator (2), characterized in that: An intermediate separator is provided between the filter press (1) and the phase separator (2), the intermediate separator comprising an intermediate separation tank (3) and a cyclone separation tank (4), an inner separation cylinder (301) with a top seal is installed through the upper portion of the intermediate separation tank (3), a filter screen (302) is installed at the lower portion of the inner separation cylinder (301), a spiral slag discharger (303) extending to the outside of the intermediate separation tank (3) is installed on the inner separation cylinder (301) above the filter screen (302), the slag discharge ports of the filter press (1) and the spiral slag discharger (303) are both connected to a slag storage tank (6) via a slag discharge pipe (5), and the cyclone separation tank (4) is installed in the intermediate separation tank (3). Above the inner separation cylinder (301) and in communication therewith, a spiral cyclone groove is provided on the inner wall of the cyclone separation tank (4), a liquid guide port (401) is tangentially installed on the upper portion of the cyclone separation tank (4), the liquid guide port (401) is in communication with the liquid outlet of the filter press (1) through a first communicating pipe (7), the top outlet of the cyclone separation tank (4) is in communication with the liquid inlet of the phase separator (2) through a second communicating pipe (8), the high-boiling-material outlet of the phase separator (2) is connected to a high-boiling-material storage tank (9), and the acid outlets of the intermediate separation tank (3) and the phase separator (2) are both connected to a hydrochloric acid storage tank (11) through an acid discharge pipe (10).

2. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 1, characterized in that: The filter press (1) comprises an outer shell (101) and a filter cartridge (102) fixedly mounted in the outer shell (101); a sealing plate (103) is mounted on the feed end of the filter cartridge (102); a discharge end of the filter cartridge (102) is an open structure; a feed pipe (104) extending to the top of the outer shell is arranged at the top of the filter cartridge (102) near one end of the sealing plate (103); a spiral extrusion shaft (105) is coaxially mounted inside the filter cartridge (102); a feed rotating shaft (106) is mounted at one end of the spiral extrusion shaft (105); the feed rotating shaft (106) passes through the sealing plate (103) and rotates to install the filter cartridge (102). The outer shell (101) is mounted on one end of the outer shell (101). A driving motor (107) connected to a feed shaft (106) is mounted on the outer shell (101). A discharge shaft (108) is mounted on the other end of the screw extrusion shaft (105). The discharge shaft (108) is rotatably mounted on the other end of the outer shell (101). A slag receiving hopper (109) is mounted on the outer shell (101) below the discharge end of the filter press cylinder (102). The slag discharge port is arranged at the bottom of the slag receiving hopper (109). A plurality of liquid leakage holes (110) are arranged at the bottom of the filter press cylinder (102). The liquid outlet is arranged at the bottom of the outer shell (101).

3. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 2, characterized in that: The bottom of the outer shell (101) is arranged in a structure with high ends and a low middle, and the liquid outlet is arranged in the middle of the outer shell (101).

4. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 2, characterized in that: A gauze is provided in the liquid leakage hole (110).

5. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 2, characterized in that: The diameter of the spiral extrusion shaft (105) gradually increases from the feed end to the discharge end.

6. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 1, characterized in that: The filter screen (302) is arranged obliquely in the inner separation cylinder (301), the spiral slag discharger (303) is arranged in coordination with the filter screen (302), and the slag discharge port of the spiral slag discharger (303) is arranged on one side of the lower end of the filter screen (302).

7. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 1, characterized in that: An overflow port (304) is provided at the top of the intermediate separation tank (3), an overflow tank body (305) is installed in a sealed manner on the outside of the intermediate separation tank (3) outside the overflow port (304), and a bypass pipe (306) communicating with the second connecting pipe (8) is provided at the bottom of the overflow tank body (305).

8. The efficient recovery system for high-boiling substances in organosilicon slurry according to claim 1, characterized in that: A plurality of baffles (307) are staggeredly installed in the inner separation cylinder (301) above the spiral slag discharger (303). The baffles (307) are arranged in an inclined downward direction in the inner separation cylinder (301).

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