CN214780792U

CN214780792U - Useless active alumina processing system

Info

Publication number: CN214780792U
Application number: CN202121265868.6U
Authority: CN
Inventors: 刘�文
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-06-04
Filing date: 2021-06-04
Publication date: 2021-11-19
Anticipated expiration: 2031-06-04

Abstract

The utility model belongs to the technical field of waste resource is recycled, concretely relates to useless active alumina processing system, including sodium carbonate preparation jar and cooking kettle, sodium carbonate preparation jar is connected with cooking kettle, the last waste alumina feed inlet that is equipped with of cooking kettle, cooking kettle's liquid outlet and layering cauldron are connected, cooking kettle's bin outlet and calcination workshop are connected, the liquid outlet of layering is connected with regeneration reactor through multistage washing kettle, regeneration reactor is connected with the distillation column, the distillation column discharge gate is connected with centrifuge, centrifuge is connected with the rectifying column, layering kettle's bottom bin outlet is connected with the pressure filter, the bin outlet and the calcination workshop of pressure filter are connected, the liquid outlet and the distillation kettle of pressure filter are connected, distillation kettle's discharge gate and drying chamber are connected. The utility model discloses can carry out high-efficient processing with useless alumina, with the effectual recovery that retrieves of alumina, can carry out thorough recovery with products such as anthraquinones wherein simultaneously, whole processing technology does not have the production of waste material basically, can be with material recycle.

Description

Useless active alumina processing system

Technical Field

The utility model belongs to the technical field of waste resource recycles, concretely relates to useless active alumina processing system.

Background

The main method for industrially producing hydrogen peroxide at present is an anthraquinone method, wherein 2-ethyl anthraquinone and tetrahydro-2-ethyl anthraquinone are used as carriers (the total effective anthraquinone content is 130-140 g/L) and heavy aromatic hydrocarbon and trioctyl phosphate (TOP) are used as mixed solvents (the volume ratio is 75:25) to prepare working solution. The working solution and hydrogen gas are fed into a fixed bed containing a palladium catalyst, and hydrogenation reaction is carried out under the pressure of 0.27-0.30 MPa (G) and the temperature of 40-70 ℃ to obtain corresponding hydroanthraquinone solution (called hydrogenated liquid). Oxidizing the hydrogenated liquid by air in an oxidation tower under the conditions of 0.22-0.3 MPa (G) pressure and 45-55 ℃, and reducing the hydroanthraquinone in the hydrogenated liquid into the original anthraquinone and simultaneously generating hydrogen peroxide. Because the solubility of hydrogen peroxide in water and working solution is different, pure water is used for extracting working solution (called oxidation solution) containing hydrogen peroxide to obtain 27.5% hydrogen peroxide aqueous solution (called extraction solution), the extraction solution is purified by heavy aromatics to remove soluble organic impurities to obtain a finished product, the extracted oxidation solution is called raffinate, the raffinate is firstly separated from most of water by a raffinate separator, then dried by potassium carbonate solution to remove water, decompose hydrogen peroxide and neutralize acid in the oxidation process, the dried working solution is settled and separated to remove entrained potassium carbonate solution, and then activated alumina in a white soil bed is subjected to post-treatment to adsorb to regenerate the working solution and remove potassium carbonate and byproducts, so that the working solution is regenerated into fresh working solution for recycling. In the hydrogenation process, part of 2-ethyl anthraquinone is converted into tetrahydro 2-ethyl hydrogen anthraquinone, the tetrahydro 2-ethyl anthraquinone is obtained after oxidation, and can be repeatedly hydrogenated and oxidized to generate hydrogen peroxide, and the existence of a certain amount of tetrahydro 2-ethyl anthraquinone is beneficial to improving the hydrogenation reaction speed and inhibiting the generation of other byproducts.

In the reaction process of the 2-ethyl anthraquinone, except physical loss, due to organic reaction, activity and selectivity of a palladium catalyst and other reasons, an unwanted byproduct (anthraquinone degradation product) is generated along with side reaction, so that the effective anthraquinone content is reduced, the physical property of the working solution is changed when the content is high, and the system cannot run when the content is serious.

The activated alumina has the function of regenerating anthraquinone degradation products in the hydrogenated liquid, can adsorb moisture and post-treated alkali liquor, and improves the quality of the working liquid. Along with the increase of the service time, the performance of the activated alumina is reduced, and in order to ensure the efficient operation of the system, the activated alumina needs to be replaced according to the system condition.

At present, the replaced waste alumina is determined as dangerous waste, and the waste alumina is discharged out of the system after the hydrogen peroxide is produced and used, wherein the waste alumina contains a large amount of alumina, partial organic matters (2-ethyl anthraquinone, tetrahydro 2-ethyl anthraquinone and trioctyl phosphate), water and a small amount of trace elements. The waste alumina is judged to be hazardous waste mainly due to the presence of organic matter. Most of the waste alumina is incinerated, and because the waste alumina contains a large amount of organic matters, the waste alumina can cause VOCS tail gas to seriously pollute the environment after incineration, and the organic matters in the waste alumina are wasted and lost.

The recovery method of the waste activated alumina in the process of producing hydrogen peroxide by the 2019103614544 anthraquinone method applied by the applicant solves the technical problems, but the recovery efficiency is still insufficient in the production.

SUMMERY OF THE UTILITY MODEL

The to-be-solved technical problem of the utility model is: the defects of the prior art are overcome, the waste activated alumina treatment system is provided, waste alumina can be efficiently treated, alumina is effectively recycled, products such as anthraquinone can be thoroughly recycled, and the waste of resources is avoided.

The utility model discloses an adopt following technical scheme to realize:

the waste activated alumina treatment system comprises a sodium carbonate preparation tank and a cooking kettle, wherein the sodium carbonate preparation tank is connected with the cooking kettle, a waste alumina feeding hole is formed in the cooking kettle, the top of the cooking kettle is connected with an adsorption tower through a first condenser, a liquid outlet of the cooking kettle is connected with a layering kettle, a discharge hole of the cooking kettle is connected with a roasting workshop, the layered liquid outlet is connected with a regeneration reactor through a multistage washing kettle, the regeneration reactor is connected with a distillation tower, the top of the distillation tower is connected with the adsorption tower through first condensing equipment, a discharge hole of the distillation tower is connected with a centrifugal machine, the centrifugal machine is connected with a rectifying tower, and the top of the rectifying tower is connected with the adsorption tower through second condensing equipment; the bottom bin outlet and the pressure filter of layering cauldron are connected, and the bin outlet and the calcination workshop of pressure filter are connected, and the liquid outlet and the stills of pressure filter are connected, and the stills top is connected with the adsorption tower through the fourth condenser, and stills's discharge gate and drying chamber are connected, and the drying chamber top is connected with the adsorption tower through the fifth condenser, be equipped with defroster and molecular sieve packing layer in the adsorption tower.

Wherein:

preferably, the first condenser is connected with the digesting tank for refluxing.

Preferably, multistage washing cauldron is equipped with the phosphoric acid inlet pipe including the primary washing cauldron, secondary washing cauldron and the cubic washing cauldron that connect gradually on the secondary washing cauldron, be equipped with the pure water moisturizing pipe on the cubic washing cauldron, and the outlet and the primary washing cauldron of secondary washing cauldron are connected, and the outlet and the secondary washing cauldron of cubic washing cauldron are connected.

Preferably, the liquid outlet of the first condensing equipment is connected with the layering kettle.

Preferably, the first condensing device comprises a second condenser and a first cryogenic condenser connected in series.

Preferably, the second condensing device comprises a third condenser and a second cryogenic condenser connected in series.

Preferably, the waste molecular sieve outlet of the adsorption tower is connected with the waste alumina feed inlet.

Preferably, the demisting water outlet of the adsorption tower is connected with the sodium carbonate preparation tank.

Preferably, the liquid outlet of the fourth condenser is connected with a sodium carbonate preparation tank.

Preferably, the liquid outlet of the fifth condenser is connected with a sodium carbonate preparation tank.

Compared with the prior art, the beneficial effects of the utility model are as follows:

the utility model discloses can carry out high-efficient processing with useless active alumina, with the effectual recovery that retrieves of alumina, can carry out thorough recovery with products such as anthraquinone wherein simultaneously, whole processing technology does not have the production of waste material basically, can use material circulation, has avoided the waste of resource, has reduced the cost for the enterprise and has improved the benefit.

Drawings

Fig. 1 is a schematic structural view of the present invention;

in the figure: 1. a sodium carbonate preparation tank; 2. a cooking kettle; 3. a waste alumina feed inlet; 4. a first condenser; 5. layering a kettle; 6. washing the kettle with water for the first time; 7. a phosphoric acid feeding pipe; 8. washing the kettle with water for the second time; 9. a pure water replenishing pipe; 10. washing the kettle with water for the third time; 11. a regeneration reactor; 12. a distillation column; 13. a centrifuge; 14. a second condenser; 15. a first cryogenic condenser; 16. a rectifying tower; 17. a third condenser; 18. a second cryogenic condenser; 19. an adsorption tower; 20. a demister; 21. a molecular sieve packing layer; 22. a fifth condenser; 23. a drying chamber; 24. a fourth condenser; 25. a distillation kettle; 26. a filter press; 27. and (4) a roasting workshop.

Detailed Description

The present invention will be further described with reference to the accompanying drawings.

As shown in fig. 1, the waste activated alumina treatment system comprises a sodium carbonate preparation tank 1 and a cooking kettle 2, wherein the sodium carbonate preparation tank 1 is connected with the cooking kettle 2, a waste alumina feed inlet 3 is arranged on the cooking kettle 2, the top of the cooking kettle 2 is connected with an adsorption tower 19 through a first condenser 4, a liquid outlet of the cooking kettle 2 is connected with a layered kettle 5, a discharge outlet of the cooking kettle 2 is connected with a roasting workshop 27, a liquid outlet of the layered kettle 5 is connected with a regeneration reactor 11 through a multi-stage washing kettle, the regeneration reactor 11 is connected with a distillation tower 12, the top of the distillation tower 12 is connected with the adsorption tower 19 through a first condensing device, a discharge outlet of the distillation tower 12 is connected with a centrifuge 13, the centrifuge 13 is connected with a rectifying tower 16, and the top of the rectifying tower 16 is connected with the adsorption tower 19 through a second condensing device; the bottom bin outlet and the pressure filter 26 of layering cauldron 5 are connected, and the bin outlet and the calcination workshop 27 of pressure filter 26 are connected, and the liquid outlet and the stills 25 of pressure filter 26 are connected, and stills 25 top is connected with adsorption tower 19 through fourth condenser 24, and stills 25's discharge gate is connected with drying chamber 23, and drying chamber 23 top is connected with adsorption tower 19 through fifth condenser 22, be equipped with defroster 20 and molecular sieve packing layer 21 in the adsorption tower 19.

The first condenser 4 is connected with the cooking kettle 2. Multistage washing cauldron is equipped with phosphoric acid inlet pipe 7 including the primary washing cauldron 6, secondary washing cauldron 8 and the cubic washing cauldron 10 that connect gradually on the secondary washing cauldron 8, be equipped with pure water moisturizing pipe 9 on the cubic washing cauldron 10, and the outlet and the primary washing cauldron 6 of secondary washing cauldron 8 are connected, and the outlet and the secondary washing cauldron 8 of cubic washing cauldron 10 are connected. The liquid outlet of the first condensing equipment is connected with the layering kettle 5. The first condensing device includes a second condenser 14 and a first cryogenic condenser 15 connected in series. The second condensing device includes a third condenser 17 and a second cryogenic condenser 18 connected in series. The waste molecular sieve outlet of the adsorption tower 19 is connected with the waste alumina feed inlet 3. The demisting water outlet of the adsorption tower 19 is connected with the sodium carbonate preparation tank 1. The liquid outlet of the fourth condenser 24 is connected with the sodium carbonate preparation tank 1. The liquid outlet of the fifth condenser 22 is connected with the sodium carbonate preparation tank 1.

When in work, the method specifically comprises the following steps:

(1) preparing alkali liquor, preparing 5.67 wt% of sodium carbonate solution, then putting waste aluminum oxide into the sodium carbonate solution for cooking, recovering the cooked aluminum oxide after roasting treatment after cooking, layering cooking liquor after cooking, and feeding gas phase generated by cooking into an adsorption tower for adsorption after condensation and reflux;

(2) carrying out three-stage water washing on the upper-layer solution of the layered cooking liquor, adding 75% phosphoric acid to remove potassium carbonate and sodium carbonate in the water washing process, then regenerating, carrying out negative pressure distillation on the regenerated solution to remove heavy aromatic hydrocarbon, reusing the heavy aromatic hydrocarbon in the layered solution, allowing the noncondensable gas subjected to negative pressure distillation and condensation to enter an adsorption tower for adsorption, centrifuging to remove trioctyl phosphate (TOP), carrying out negative pressure rectification treatment, reusing the front fraction subjected to negative pressure rectification in the layered solution, condensing the recovered fraction to obtain an anthraquinone product, and allowing the noncondensable gas subjected to condensation to enter the adsorption tower for adsorption;

(3) and (3) carrying out filter pressing on the lower-layer solution of the layered cooking liquor, recovering the aluminum oxide obtained by filter pressing after roasting treatment, distilling the filtrate obtained by filter pressing, drying the heavy component obtained by distillation, condensing the light component generated by distillation and drying, then feeding the light component into an adsorption tower for adsorption, and recycling the condensed condensate for preparing the sodium carbonate solution.

Wherein, be equipped with molecular sieve and defroster in the adsorption tower, waste molecular sieve after the adsorption treatment puts into sodium carbonate solution together with useless alumina and carries out the boiling treatment, and the defogging water that the defroster produced is used for sodium carbonate solution preparation again.

Of course, the above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and the technical field of the present invention is equivalent to the changes and improvements made in the actual range of the present invention, which should be attributed to the patent coverage of the present invention.

Claims

1. A waste activated alumina processing system, characterized in that: comprises a sodium carbonate preparation tank (1) and a cooking kettle (2), wherein the sodium carbonate preparation tank (1) is connected with the cooking kettle (2), a waste alumina feeding port (3) is arranged on the cooking kettle (2), the top of the cooking kettle (2) is connected with an adsorption tower (19) through a first condenser (4), a liquid outlet of the cooking kettle (2) is connected with a layering kettle (5), a discharge port of the cooking kettle (2) is connected with a roasting workshop (27), a liquid outlet of the layering kettle (5) is connected with a regeneration reactor (11) through a multi-stage washing kettle, the regeneration reactor (11) is connected with a distillation tower (12), the top of the distillation tower (12) is connected with an adsorption tower (19) through first condensing equipment, a discharge port of the distillation tower (12) is connected with a centrifugal machine (13), the centrifugal machine (13) is connected with a rectifying tower (16), and the top of the rectifying tower (16) is connected with the adsorption tower (19) through second condensing equipment; the bottom bin outlet of layering cauldron (5) is connected with pressure filter (26), and the bin outlet and roasting workshop (27) of pressure filter (26) are connected, and the liquid outlet and stills (25) of pressure filter (26) are connected, and stills (25) top is connected with adsorption tower (19) through fourth condenser (24), and the discharge gate and drying chamber (23) of stills (25) are connected, and drying chamber (23) top is connected with adsorption tower (19) through fifth condenser (22), be equipped with defroster (20) and molecular sieve packing layer (21) in adsorption tower (19).

2. The spent activated alumina treatment system of claim 1, wherein: the first condenser (4) is connected with the cooking kettle (2).

3. The spent activated alumina treatment system of claim 1, wherein: multistage washing kettle is equipped with phosphoric acid inlet pipe (7) including the primary washing cauldron (6), secondary washing cauldron (8) and cubic washing cauldron (10) that connect gradually on secondary washing cauldron (8), be equipped with pure water moisturizing pipe (9) on cubic washing cauldron (10), and the outlet and the primary washing cauldron (6) of secondary washing cauldron (8) are connected, and the outlet and the secondary washing cauldron (8) of cubic washing cauldron (10) are connected.

4. The spent activated alumina treatment system of claim 1, wherein: the liquid outlet of the first condensing equipment is connected with the layering kettle (5).

5. The spent activated alumina treatment system according to claim 1 or 4, wherein: the first condensing equipment comprises a second condenser (14) and a first cryogenic condenser (15) which are connected in sequence.

6. The spent activated alumina treatment system of claim 1, wherein: the second condensing equipment comprises a third condenser (17) and a second cryogenic condenser (18) which are connected in sequence.

7. The spent activated alumina treatment system of claim 1, wherein: the waste molecular sieve outlet of the adsorption tower (19) is connected with the waste alumina feed inlet (3).

8. The spent activated alumina treatment system of claim 1, wherein: the demisting water outlet of the adsorption tower (19) is connected with the sodium carbonate preparation tank (1).

9. The spent activated alumina treatment system of claim 1, wherein: the liquid outlet of the fourth condenser (24) is connected with the sodium carbonate preparation tank (1).

10. The spent activated alumina treatment system of claim 1, wherein: the liquid outlet of the fifth condenser (22) is connected with the sodium carbonate preparation tank (1).