CN214612688U - Equipment for extracting titanium liquid from olefin polymerization industrial waste acid residues - Google Patents
Equipment for extracting titanium liquid from olefin polymerization industrial waste acid residues Download PDFInfo
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- CN214612688U CN214612688U CN202023155230.5U CN202023155230U CN214612688U CN 214612688 U CN214612688 U CN 214612688U CN 202023155230 U CN202023155230 U CN 202023155230U CN 214612688 U CN214612688 U CN 214612688U
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Abstract
The utility model discloses an equipment for extracting titanium liquid from olefin polymerization industry acid sludge, the equipment includes normal atmospheric temperature normal pressure hydrolysis system, ozone catalytic oxidation system, middle filtration system, aqueous ammonia neutralization and add magnesium dephosphorization desiliconization system, tubular microfiltration membrane system. The utility model discloses titanium can be retrieved in a large number from olefin polymerization industry waste acid sludge to equipment, and the technology operation requires that low, the rate of recovery is high, the accessory substance of production is few, friendly to the environment, has wide industrial application prospect.
Description
Technical Field
The utility model belongs to the technical field of petrochemical, especially, relate to the recovery of titanium tetrachloride among the industrial production of olefin polymerization catalyst, specifically be an equipment of extracting high-purity titanium liquid from olefin polymerization industry waste acid sludge.
Background
Titanium tetrachloride is an important and largely used raw material in the industrial production of olefin polymerization catalysts, and a large amount of titanium tetrachloride-containing waste liquid is produced after use. The waste liquid contains a large amount of unreacted titanium tetrachloride and a certain amount of related byproducts such as alkoxy titanium (containing chlorine), ester titanium complex and other organic solvents. COD, TOC and Ga in wastewater2+、Mg2+Ti ion, total phosphorus, soluble silicon, Cl-Very high TDS values, very complex compositions. Wherein Ti has the highest recycling value.
There are two prior art treatments. The first method is to add the acid sludge into the quicklime for neutralization reaction to produce a large amount of precipitate, and then separate the precipitate by using a plate-and-frame filter press. Valuable titanium cannot be recovered by plate and frame filter pressing. The second method is to directly adopt a high-temperature evaporation process to the waste acid residues to evaporate hydrochloric acid in the waste acid residues, titanium oxide crystals can be generated at the bottom of an evaporation kettle, but the requirement on corrosion resistance of equipment is extremely high due to the fact that the evaporation kettle works in a hydrochloric acid environment, and batch production and long-period operation are difficult to achieve. Moreover, the second method has the following problems: the high temperature of the bottom of the distillation tower causes decomposition, coking and fouling of organic matters such as alkoxy titanium, ester titanium complex and the likeIn order to facilitate the discharge of the bottom, it is necessary to control the evaporation temperature and to leave a certain quantity of TiCl4. Thus greatly reducing TiCl4The recovery rate is increased, and the amount of waste is increased. And a large amount of acid water, acid gas and waste residues are generated when the waste is reprocessed, so that the waste is not easy to treat and pollutes the environment.
Disclosure of Invention
The utility model aims to overcome prior art's defect, provide an equipment of extracting high-purity titanium liquid from olefin polymerization industry waste acid sediment, use this equipment can realize hydrolysising, ozone catalytic oxidation, add ammonia and magnesium and get rid of phosphate radical and silicic acid radical and tubular membrane filterable technology operation, and then obtain high-purity Ti (OH)4The solution realizes the purpose of resource treatment of the waste acid sludge.
The purpose of the utility model is realized like this:
a device for extracting high-purity titanium liquid from olefin polymerization industrial waste acid residues comprises a normal-temperature normal-pressure hydrolysis system, an ozone catalytic oxidation system, an intermediate filtering system, an ammonia water neutralization and magnesium-adding phosphorus and silicon removal system and a tubular microfiltration membrane system; the normal temperature and normal pressure hydrolysis system comprises a primary hydrolysis system and a secondary hydrolysis system; the liquid outlet end of the normal temperature and normal pressure system is connected to the liquid inlet end of the ozone catalytic oxidation system through a water pump and a hydrolysis supernatant liquid output pipeline; the liquid outlet end of the ozone catalytic oxidation system is connected to the liquid inlet end of the intermediate filtering system through a pipeline; the liquid outlet end of the intermediate filtering system is connected to the liquid inlet end of the ammonia water neutralization and magnesium addition phosphorus and silicon removal system through a pipeline; the liquid outlet end of the ammonia water neutralization and magnesium addition dephosphorization and desilicification system is connected to the liquid inlet end of the tubular microfiltration membrane system through a pipeline.
According to a further optimization scheme, the normal-temperature and normal-pressure hydrolysis system comprises a primary hydrolysis system, a secondary hydrolysis system, a waste acid residue collecting system, a filter pressing system, a hydrolysis supernatant collecting device, a clear water inlet pipe and a waste acid residue feeding device; the primary hydrolysis system comprises: a primary hydrolysis tank, a primary hydrolysis circulating pump and a primary hydrolysis output pump; the secondary hydrolysis system comprises: a secondary hydrolysis tank, a secondary hydrolysis circulating pump and a secondary hydrolysis output pump; the waste acid sludge collecting system comprises: a sludge tank and a sludge feed pump; the primary hydrolysis tank and the secondary hydrolysis tank are respectively provided with a waste acid residue inlet, a waste acid residue and circulating water outlet, a liquid inlet, a hydrolysis supernatant outlet and a circulating water inlet; a waste acid residue inlet of the primary hydrolysis tank is connected with the waste acid residue feeding device; the liquid inlet of the first-stage hydrolysis tank is connected to the clear water inlet pipe through a branch pipeline, and a water inlet valve of the first-stage hydrolysis tank is arranged on the branch pipeline; the waste acid sludge and circulating water outlet of the first-stage hydrolysis tank is connected to the water inlet end of the first-stage hydrolysis circulating pump through a pipeline, the water outlet end pipeline of the first-stage hydrolysis circulating pump is divided into two branch pipelines which are respectively connected to the circulating water inlet of the first-stage hydrolysis tank and the waste acid sludge inlet of the second-stage hydrolysis tank, wherein the branch pipeline connected with the circulating water inlet of the first-stage hydrolysis tank is provided with a first-stage hydrolysis tank inlet circulating valve, and the branch pipeline connected with the waste acid sludge inlet of the second-stage hydrolysis tank is provided with a first-stage hydrolysis tank outlet discharge valve; a supernatant outlet of the primary hydrolysis tank is connected to a water inlet end of the primary hydrolysis outward-conveying pump, and a water outlet pipeline of the primary hydrolysis outward-conveying pump is connected to a hydrolysis supernatant collecting device; the liquid inlet of the secondary hydrolysis tank is connected to the clear water inlet pipe through a branch pipeline, and a water inlet valve of the secondary hydrolysis tank is arranged on the branch pipeline; the waste acid sludge and circulating water outlet of the second-stage hydrolysis tank is connected to the water inlet end of a second-stage hydrolysis circulating pump through a pipeline, the water outlet end pipeline of the second-stage hydrolysis circulating pump is divided into two branch pipelines which are respectively connected to the circulating water inlet of the second-stage hydrolysis tank and the inlet of the sludge tank, wherein a second-stage hydrolysis tank inlet circulating valve is arranged on the branch pipeline connected with the circulating water inlet of the second-stage hydrolysis tank, and a second-stage hydrolysis tank outlet discharge valve is arranged on the branch pipeline connected with the inlet of the sludge tank; a supernatant outlet of the secondary hydrolysis tank is connected to a water inlet end of the secondary hydrolysis outward-conveying pump, and a water outlet pipeline of the secondary hydrolysis outward-conveying pump is connected to a hydrolysis supernatant collecting device; the export of sludge case passes through the feed end of tube coupling mud feed pump, and the discharge end of mud feed pump passes through tube coupling to filter-pressing system, and filter-pressing system's filtrating discharge line inserts the second grade case of hydrolysising.
Further, the ozone catalytic oxidation system comprises an ozone reaction tower, an ozone generator, an ozone destructor and an oxidation water production tank; the top of the ozone reaction tower is provided with an ozone destructor, the inside of the ozone reaction tower is provided with an upper layer of clapboard with holes and a lower layer of clapboard with holes, a catalyst packing layer is arranged between the two layers of clapboards, the bottom of the ozone reaction tower is fixed with an air duct, the air duct is provided with a plurality of micron bubble aeration heads, and an air inlet interface of the air duct is connected with an air duct of the ozone generator; a hydrolysis supernatant inlet is arranged on the side wall of the ozone reaction tower and positioned below the catalyst packing layer, and the hydrolysis supernatant inlet is connected to a hydrolysis liquid outlet end of the normal-temperature normal-pressure hydrolysis system through a pipeline; a water outlet after reaction is arranged on the side wall of the ozone reaction tower above the catalyst packing layer and is connected with a water inlet of the oxidation water production tank through a pipeline; the middle filtering system comprises a filter and a filter water feeding pump connected with the filter, a water outlet of the oxidation product water tank is connected with a water inlet end of the filter water feeding pump through a pipeline, a water outlet end of the filter water feeding pump is connected with a water inlet end of the filter, and a water outlet end of the filter is connected with the ammonia water neutralizing and magnesium adding phosphorus and silicon removing system; the ammonia water neutralization and magnesium-adding phosphorus and silicon removal system comprises an ammonia water neutralization tank, a phosphorus and silicon removal tank, a neutralization sludge discharge pump, an ammonia water feeding device and a magnesium agent feeding device, wherein the phosphorus and silicon removal tank is communicated with the ammonia water neutralization tank, the bottom of the phosphorus and silicon removal tank is conical, a water inlet of the ammonia water neutralization tank is connected with a water outlet end of the filter, the ammonia water neutralization tank is connected with the phosphorus and silicon removal tank through an overflow port, the bottom of the phosphorus and silicon removal tank is provided with a precipitation outlet and is connected to the neutralization sludge discharge pump through a pipeline, the side wall of the phosphorus and silicon removal tank is provided with a titanium hydroxide suspension overflow port, and the titanium hydroxide suspension overflow port is connected to the tubular microfiltration membrane system; the ammonia water adding device comprises an ammonia water storage tank and an ammonia water dosing pump, wherein the liquid outlet end of the ammonia water storage tank is connected with the liquid inlet end of the ammonia water dosing pump, and the liquid outlet end of the ammonia water dosing pump is connected to the liquid inlet pipeline of the ammonia water neutralizing tank; the magnesium agent feeding device comprises a magnesium agent feeding box and a magnesium agent feeding pump, the liquid outlet end of the magnesium agent feeding box is connected with the liquid inlet end of the magnesium agent feeding pump, and the liquid outlet end of the magnesium agent feeding pump is connected to the liquid inlet pipeline of the ammonia water neutralizing box.
The tubular microfiltration membrane system comprises a tubular membrane water feeding pump, a tubular membrane circulating pump, a tubular membrane device, a tubular membrane water production tank, a neutralization water pump, a titanium hydroxide feed liquid tank, a tubular membrane cleaning device and an automatic control device; the liquid inlet end of the tubular membrane water feeding pump is connected with a titanium hydroxide suspension overflow port of the phosphorus and silicon removing tank through a pipeline, the liquid outlet end of the tubular membrane water feeding pump is connected with the liquid inlet end of the tubular membrane circulating pump, the liquid outlet end of the tubular membrane circulating pump is connected with the liquid inlet of the tubular membrane device, the concentrated liquid outlet of the tubular membrane device is connected to a titanium hydroxide material liquid tank through a pipeline, a material liquid control valve is arranged on the pipeline between the concentrated liquid outlet of the tubular membrane device and the titanium hydroxide material liquid tank, and the pipeline between the material liquid control valve and the concentrated liquid outlet of the tubular membrane device is communicated with the pipeline between the tubular membrane water feeding pump and the tubular membrane circulating pump through a branch pipeline; a product water outlet of the tubular membrane device is connected to a liquid inlet end of the tubular membrane water production tank through a product water outlet pipeline, a product water control valve is arranged on the product water outlet pipeline, a liquid outlet end of the tubular membrane water production tank is connected to a liquid inlet end of a neutralization water pump, and a liquid outlet end of the neutralization water pump is connected with a neutralization device; and the automatic control device is electrically connected with the tubular membrane water feeding pump, the tubular membrane circulating pump, the neutralizing water pump and the water pump in the tubular membrane cleaning device to control the work of each water pump.
Further, the tubular membrane cleaning device comprises a tubular membrane backwashing pump and a chemical cleaning device, wherein the chemical cleaning device comprises a tubular membrane cleaning water tank and a tubular membrane cleaning pump; the liquid outlet end of the tubular membrane water production tank is provided with a branch pipeline connected with the liquid inlet end of the tubular membrane backwashing pump, the liquid outlet end of the tubular membrane backwashing pump is connected with the product water outlet pipeline of the tubular membrane device, and the connection point is positioned between the product water outlet of the tubular membrane device and the product water control valve; the liquid outlet of the tubular membrane cleaning water tank is connected with the liquid inlet end of the tubular membrane cleaning pump, the liquid outlet end of the tubular membrane cleaning pump is connected to a liquid inlet pipeline between the tubular membrane circulating pump and the liquid inlet of the tubular membrane device through a pipeline, and a branch pipeline is respectively branched from the concentrated solution outlet and the product water outlet of the tubular membrane device and connected to the liquid inlet of the tubular membrane cleaning water tank.
The utility model has the advantages and beneficial effects that: use the utility model discloses equipment can follow and retrieve titanium in a large number in the olefin polymerization industry acid sludge, this equipment operation requires low, the rate of recovery is high, equipment fixing and maintenance are simple and convenient, the accessory substance of production is few, friendly to the environment, has wide industrial application prospect.
Drawings
The present invention will be further explained with reference to the drawings and examples.
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of a normal temperature and pressure hydrolysis device for waste acid sludge according to the embodiment of the present invention;
FIG. 3 is a schematic view of an apparatus for removing phosphorus and silicon by catalytic oxidation of ozone and adding magnesium and ammonia water according to an embodiment of the present invention;
FIG. 4 is a schematic view of a tubular microfiltration membrane titanium solution concentration apparatus according to an embodiment of the present invention;
FIG. 5 is a schematic view of the structure of an ozone reaction tower in the example.
Reference numerals: 1-1, a first-stage hydrolysis tank; 1-2, a first-stage hydrolysis circulating pump; 1-3, a first-stage hydrolysis output pump; 1-4. a water inlet valve of a first-stage hydrolysis tank; 1-5, an inlet circulating valve of the first-stage hydrolysis tank; 1-6, outlet discharge valve of first-stage hydrolysis pump; 2-1, a secondary hydrolysis tank; 2-2, a second-stage hydrolysis circulating pump; 2-3, a secondary hydrolysis output pump; 2-4, a water inlet valve of the secondary hydrolysis tank; 2-5, circulating valve at inlet of secondary hydrolysis tank; 2-6, secondary hydrolysis pump outlet discharge valve; 3-1, a sludge box; 3-2, a sludge feeding pump; 3-3, circulating valve of sludge pump outlet; 3-4, a sludge discharge valve; 4-1, plate and frame filter press; 4-2, a filtrate water tank; 4-3, a filtrate water pump; 5. a hydrolysis supernatant collecting device; 5-1, an output pump; -2. discharging the hydrolysis supernatant; 6. a clear water inlet pipe; 7. a waste acid sludge feeding device; 8-1, an ozone reaction tower; 8-2. an ozone generator; 8-3, ozone destructor; 8-4, oxidizing the water producing tank; 8-5, a separator; 8-6, ventilating pipeline; 8-7. micron bubble aeration head; 8-8, feeding hydrolysis supernatant; 8-9, water outlet after reaction; 9-1. a filter; 9-2. a water pump of the filter; 10-1, an ammonia water neutralizing tank; 10-2, a phosphorus and silicon removing box; 10-3, neutralizing the dredge pump; 10-4, an ammonia water storage tank; 10-5, ammonia water dosing pump; 10-6. a cosmetic agent feeding box; 10-7, a magnesium agent dosing pump; 10-8, titanium hydroxide suspension; 11-1. a tubular membrane feed pump; 11-2. a tubular membrane circulating pump; 11-3. a tubular membrane device; 11-4. a tubular membrane water production tank; 11-5, a neutralization water pump; 11-6, a titanium hydroxide feed liquid box; 11-7, a tubular membrane backwashing pump; 11-8, a tubular membrane cleaning water tank; 11-9. a tubular membrane cleaning pump; 11-10, a feed liquid control valve; 11-11. tubular membrane water production control valve; 11-12. a feeding pump of the titanium hydroxide crystallizer; 11-13. producing water by the membrane; 11-14, concentrating the titanium hydroxide concentrated solution by a tubular membrane; a1. waste acid sludge inlet of the first-level hydrolysis tank; a2. a liquid inlet of the first-stage hydrolysis tank; a3. a waste acid sludge and circulating water outlet of the primary hydrolysis tank; a4. a supernatant outlet of the first-stage hydrolysis tank; a5. a circulating water inlet of the first-stage hydrolysis tank; b1. a waste acid residue inlet of the secondary hydrolysis tank; b2. a liquid inlet of the first-stage hydrolysis tank; b3. a waste acid sludge and circulating water outlet of the primary hydrolysis tank; b4. a supernatant outlet of the first-stage hydrolysis tank; b5. a circulating water inlet of the first-stage hydrolysis tank; c1. the material circulation inlet of the sludge box.
Detailed Description
The first embodiment is as follows:
as shown in figure 1, the equipment for extracting the high-purity titanium liquid from the olefin polymerization industrial waste acid sludge comprises a normal-temperature normal-pressure hydrolysis system, an ozone catalytic oxidation system, an intermediate filtration system, an ammonia water neutralization and magnesium-adding phosphorus and silicon removal system and a tubular microfiltration membrane system; the normal temperature and normal pressure hydrolysis system comprises a primary hydrolysis system and a secondary hydrolysis system; the liquid outlet end of the hydrolysate of the normal-temperature normal-pressure hydrolysis system is connected to the liquid inlet end of the ozone catalytic oxidation system through a water pump and a hydrolysis supernatant liquid output pipeline; the liquid outlet end of the ozone catalytic oxidation system is connected to the liquid inlet end of the intermediate filtering system through a pipeline; the liquid outlet end of the intermediate filtering system is connected to the liquid inlet end of the ammonia water neutralization and magnesium addition phosphorus and silicon removal system through a pipeline; the liquid outlet end of the ammonia water neutralization and magnesium addition dephosphorization and desilicification system is connected to the liquid inlet end of the tubular microfiltration membrane system through a pipeline.
Example two:
the embodiment is a specific optimized scheme based on the first embodiment.
As shown in fig. 2, the normal temperature and pressure hydrolysis system comprises a primary hydrolysis system, a secondary hydrolysis system, a waste acid sludge collection system, a filter pressing system, a hydrolysis supernatant collection device 5, a clear water inlet pipe 6 and a waste acid sludge feeding device 7; the primary hydrolysis system comprises: a primary hydrolysis tank 1-1, a primary hydrolysis circulating pump 1-2 and a primary hydrolysis output pump 1-3; the secondary hydrolysis system comprises: a secondary hydrolysis tank 2-1, a secondary hydrolysis circulating pump 2-2 and a secondary hydrolysis output pump 2-3; the waste acid sludge collecting system comprises: 3-1 of a sludge box and 3-2 of a sludge feed pump; the primary hydrolysis tank 1-1 and the secondary hydrolysis tank 2-1 are respectively provided with a waste acid residue inlet, a waste acid residue and circulating water outlet, a liquid inlet, a supernatant outlet and a circulating water inlet;
a waste acid sludge inlet a1 (the inlet is arranged on one side above the primary hydrolysis tank) of the primary hydrolysis tank 1-1 is connected with the waste acid sludge feeding device 7 (the device can be a feeding pipe and also can be other automatic or manual feeding devices); a liquid inlet a2 of the first-stage hydrolysis tank 1-1 (the liquid inlet is arranged at the other side above the first-stage hydrolysis tank) is connected to the clean water inlet pipe 6 through a branch pipeline, and a first-stage hydrolysis tank water inlet valve 1-4 is arranged on the branch pipeline; the waste acid sludge and circulating water outlet a3 of the first-stage hydrolysis tank 1-1 (the outlet is arranged below the first-stage hydrolysis tank) is connected to the water inlet end of the first-stage hydrolysis circulating pump 1-2 through a pipeline, the water outlet end pipeline of the first-stage hydrolysis circulating pump 1-2 is divided into two branch pipelines (which can be connected by a tee joint) which are respectively connected to the circulating water inlet a5 of the first-stage hydrolysis tank 1-1 (arranged on the upper part of the side wall of the first-stage hydrolysis tank) and the waste acid sludge inlet b1 of the second-stage hydrolysis tank 2-1 (arranged on one side above the second-stage hydrolysis tank), wherein a branch pipeline connecting the water outlet end of the first-stage hydrolysis circulating pump 1-2 with the circulating water inlet a5 of the first-stage hydrolysis tank 1-1 is provided with a first-stage hydrolysis tank inlet circulating valve 1-5, a branch pipeline connected with the waste acid sludge inlet b1 of the second-stage hydrolysis tank 2-1 is provided with a discharge valve 1-6 of a first-stage hydrolysis pump outlet; a supernatant outlet a4 (arranged at the lower part of the side wall of the primary hydrolysis tank) of the primary hydrolysis tank 1-1 is connected to the water inlet end of the primary hydrolysis outward-conveying pump 1-3, and a water outlet pipeline of the primary hydrolysis outward-conveying pump 1-3 is connected to the hydrolysis supernatant collecting device 5;
a liquid inlet b2 (arranged on the other side above the secondary hydrolysis tank) of the secondary hydrolysis tank 2-1 is connected to the clear water inlet pipe 6 through a branch pipeline, and a water inlet valve 2-4 of the secondary hydrolysis tank is arranged on the branch pipeline; a waste acid sludge and circulating water outlet b3 of the second-stage hydrolysis tank 2-1 (arranged below the second-stage hydrolysis tank) is connected to the water inlet end of the second-stage hydrolysis circulating pump 2-2 through a pipeline, the water outlet end pipeline of the second-stage hydrolysis circulating pump 2-2 is divided into two branch pipelines (which can be connected by a tee joint) and respectively connected to a circulating water inlet b5 of the second-stage hydrolysis tank 2-1 (arranged at the upper part of the side wall of the second-stage hydrolysis tank) and an inlet of a sludge tank 3-1 (arranged at the upper part of the sludge tank), wherein a branch pipeline connecting the water outlet end of the second-stage hydrolysis circulating pump 2-2 with the circulating water inlet b5 of the second-stage hydrolysis tank 2-1 is provided with a second-stage hydrolysis tank inlet circulating valve 2-5, a branch pipeline connected with an inlet of the sludge tank 3-1 is provided with a secondary hydrolysis pump outlet discharge valve 2-6; a supernatant outlet b4 of the secondary hydrolysis tank 2-1 is connected to the water inlet end of the secondary hydrolysis outward delivery pump 2-3, and a water outlet pipeline of the secondary hydrolysis outward delivery pump 2-3 is connected to the hydrolysis supernatant collecting device 5;
the export of sludge box 3-1 (set up in the lower part of sludge box) passes through the feed end of tube coupling mud feed pump 3-2, and the discharge end of mud feed pump 3-2 passes through tube coupling to filter-pressing system, and filtration system includes in this embodiment: a plate-and-frame filter press 4-1 (a filter press feed valve is arranged at a feed end), a filtrate water tank 4-2 and a filtrate water pump 4-3; the discharge end of the sludge feed pump 3-2 is connected to the feed end of the plate-and-frame filter press 4-1 through a pipeline, the liquid outlet end of the plate-and-frame filter press 4-1 is connected to the inlet of the filtrate water tank 4-2 through a pipeline, the outlet of the filtrate water tank 4-2 is connected to the water inlet end of the filtrate water pump 4-3 through a pipeline, and the water outlet end of the filtrate water pump 4-3 is connected to the secondary hydrolysis tank 2-1 through a pipeline (the upper end of the side wall of the secondary hydrolysis tank is provided with an independent filtrate inlet).
In the embodiment, a liquid outlet of the hydrolysis supernatant collecting device 5 is connected to a liquid inlet end of an output pump 5-1, and a liquid outlet end of the output pump 5-1 is connected to an oxidation catalysis impurity removal system.
As shown in fig. 3, the catalytic ozonation system comprises an ozone reaction tower 8-1 (see fig. 5 for a specific structure), an ozone generator 8-2, an ozone destructor 8-3 and an oxidation water production tank 8-4; the top of an ozone reaction tower 8-1 is provided with an ozone destructor 8-3, the inside of the ozone reaction tower 8-1 is provided with an upper layer of clapboard 8-5 with holes and a lower layer of clapboard 8-5 with holes, a catalyst packing layer is arranged between the two layers of clapboards, the bottom of the ozone reaction tower 8-1 is fixed with an air duct 8-6, the air duct 8-6 is provided with a plurality of micron bubble aeration heads 8-7, and an air inlet interface of the air duct 8-6 is connected with an air duct of an ozone generator 8-2; a hydrolysis supernatant inlet 8-8 is arranged on the side wall of the ozone reaction tower 8-1 below the catalyst packing layer, the inlet is connected to the liquid outlet end of the output pump 5-1, a reacted water outlet 8-9 is arranged on the side wall of the ozone reaction tower 8-1 above the catalyst packing layer, and the reacted water outlet 8-9 is connected with a water inlet of the oxidation product water tank 8-4 through a pipeline.
The intermediate filtering system comprises a filter 9-1 and a filter water feeding pump 9-2 connected with the filter 9-1, a water outlet of the oxidation product water tank 8-4 is connected with a water inlet end of the filter water feeding pump 9-2 through a pipeline, a water outlet end of the filter water feeding pump 9-2 is connected with a water inlet end of the filter 9-1, and a water outlet end of the filter 9-1 is connected with an ammonia water neutralization and magnesium addition phosphorus and silicon removal system.
The ammonia water neutralization and magnesium adding phosphorus and silicon removal system comprises an ammonia water neutralization tank 10-1, a phosphorus and silicon removal tank 10-2, a neutralization sludge discharge pump 10-3, an ammonia water feeding device and a magnesium agent feeding device, wherein the phosphorus and silicon removal tank is communicated with the ammonia water neutralization tank, the bottom of the phosphorus and silicon removal tank is conical, a water inlet of the ammonia water neutralization tank 10-1 is connected with a water outlet end of a filter 9-1, the ammonia water neutralization tank 10-1 is connected with the phosphorus and silicon removal tank 10-2 through an overflow port, a precipitation outlet is formed in the bottom of the phosphorus and silicon removal tank 10-2 and is connected to the neutralization sludge discharge pump 10-3 through a pipeline, a titanium hydroxide suspension overflow port is formed in the side wall of the phosphorus and silicon removal tank 10-2, and the titanium hydroxide suspension overflow port is connected to the micro-filtration tubular membrane system. In the embodiment, the ammonia water adding device comprises an ammonia water storage tank 10-4 and an ammonia water dosing pump 10-5, wherein the liquid outlet end of the ammonia water storage tank 10-4 is connected with the liquid inlet end of the ammonia water dosing pump 10-5, and the liquid outlet end of the ammonia water dosing pump 10-5 is connected to the liquid inlet pipeline of the ammonia water neutralizing tank 10-1; the magnesium agent feeding device comprises a magnesium agent feeding box 10-6 and a magnesium agent feeding pump 10-7, wherein the liquid outlet end of the magnesium agent feeding box 10-6 is connected with the liquid inlet end of the magnesium agent feeding pump 10-7, and the liquid outlet end of the magnesium agent feeding pump 10-7 is connected with the liquid inlet pipeline of the ammonia water neutralizing box 10-1.
As shown in fig. 4, the tubular microfiltration membrane system comprises a tubular membrane water feed pump 11-1, a tubular membrane circulating pump 11-2, a tubular membrane device 11-3, a tubular membrane water production tank 11-4, a neutralization water pump 11-5, a titanium hydroxide feed liquid tank 11-6, a tubular membrane cleaning device and an automatic control device; the liquid inlet end of the tubular membrane water feed pump 11-1 is connected with the titanium hydroxide suspension overflow port of the phosphorus and silicon removal tank 10-2 through a pipeline, the liquid outlet end of the tubular membrane water feed pump 11-1 is connected with the liquid inlet end of the tubular membrane circulating pump 11-2, the liquid outlet end of the tubular membrane circulating pump 11-2 is connected with the liquid inlet of the tubular membrane device 11-3, the concentrated solution outlet of the tubular membrane device 11-3 is connected to a titanium hydroxide feed solution tank 11-6 through a pipeline, a feed liquid control valve 11-10 is arranged on a pipeline between the concentrated liquid outlet of the tubular membrane device 11-3 and the titanium hydroxide feed liquid tank 11-6, and a pipeline between the feed liquid control valve 11-10 and the concentrated liquid outlet of the tubular membrane device 11-3 is communicated with a pipeline between the tubular membrane water feed pump 11-1 and the tubular membrane circulating pump 11-2 through a branch pipeline; a product water outlet of the tubular membrane device 11-3 is connected to a liquid inlet end of a tubular membrane water production tank 11-4 through a product water outlet pipeline, a product water control valve 11-11 is arranged on the product water outlet pipeline, a liquid outlet end of the tubular membrane water production tank 11-4 is connected to a liquid inlet end of a neutralization water pump 11-5, and a liquid outlet end of the neutralization water pump 11-5 is connected with a neutralization device; the automatic control device is electrically connected with the tubular membrane water feeding pump 11-1, the tubular membrane circulating pump 11-2, the neutralization water pump 11-5 and the water pump in the tubular membrane cleaning device to control the work of each water pump.
The tubular membrane cleaning device comprises a tubular membrane backwashing pump 11-7 and a chemical cleaning device, wherein the chemical cleaning device comprises a tubular membrane cleaning water tank 11-8 and a tubular membrane cleaning pump 11-9; the liquid outlet end of the tubular membrane water production tank 11-4 is provided with a branch pipeline connected with the liquid inlet end of the tubular membrane backwashing pump 11-7, the liquid outlet end of the tubular membrane backwashing pump 11-7 is connected with the product water outlet pipeline of the tubular membrane device 11-3, and the connection point is positioned between the product water outlet of the tubular membrane device 11-3 and the product water control valve 11-11; the liquid outlet of the tubular membrane cleaning water tank 11-8 is connected with the liquid inlet end of the tubular membrane cleaning pump 11-9, the liquid outlet end of the tubular membrane cleaning pump 11-9 is connected with a liquid inlet pipeline between the tubular membrane circulating pump 11-2 and the liquid inlet of the tubular membrane device 11-3 through a pipeline, and a branch pipeline is respectively divided from the concentrated solution outlet and the product water outlet of the tubular membrane device 11-3 and is connected with the liquid inlet of the tubular membrane cleaning water tank 11-8.
The operation flow of the device in fig. 3 is: the hydrolysis supernatant is introduced into the bottom of an ozone reaction tower 8-1, ozone generated by an ozone generator 8-2 is sent to the bottom of the ozone reaction tower through an aeration device to react with the hydrolysis supernatant, the reacted materials flow through a catalyst in the tower and overflow to an oxidation water production tank 8-4, the liquid level of the oxidation water production tank 8-4 rises to a set liquid level value, and a filter water feeding pump 9-2 is started to convey the reacted materials to a filter 9-1; adding ammonia water into the filtrate filtered by the filter 9-1, and feeding the filtrate into an ammonia water neutralizing tank 10-1 for neutralization; adding a magnesium agent (magnesium chloride) before the filtrate filtered by the filter enters an ammonia water neutralization tank 10-1; the materials neutralized by the ammonia water neutralization tank 10-1 overflow to the phosphorus and silicon removal tank 10-2, the generated calcium phosphate, calcium silicate, magnesium silicate and the like are precipitated to the bottom of the phosphorus and silicon removal tank 10-2 and are conveyed to a sludge tank through a neutralization sludge discharge pump 10-3, and the overflowed titanium hydroxide suspension enters a tubular membrane microfiltration system.
The operation flow of the device in fig. 4 is: titanium hydroxide suspension flowing out of the phosphorus and silicon removal tank is lifted by a tubular membrane water feed pump 11-1 and then enters a tubular membrane device 11-3 for concentration, water coming from the tubular membrane water feed pump 11-1 is mixed with circulating concentrated solution and then is lifted by a tubular membrane circulating pump 11-2 to the tubular membrane device 11-3, and the concentrate of the tubular membrane device is discharged to a titanium hydroxide feed solution tank 11-6; and the product water of the tubular membrane device enters a tubular membrane water production tank 11-4 and is discharged through a neutralization water pump 11-5. The pore size of the tubular membrane filter in the tubular membrane device is 0.05 micron. The tubular membrane device 11-3 performs backwashing once by adopting a tubular membrane backwashing pump 11-7 every filtering period of time so as to recover membrane flux. Membrane systems require periodic chemical cleaning after a period of operation to restore the membrane elements to performance. After cleaning agents such as acid, alkali and the like are prepared in the tubular membrane cleaning water tank 11-8 according to a certain concentration, the cleaning agents are lifted by the tubular membrane cleaning pump 11-9 and then enter the membrane system to clean the membrane surface, and the cleaned water flows back to the tubular membrane cleaning water tank 11-8 through a pipeline for recycling.
Finally, it should be noted that the above only illustrates the technical solution of the present invention and not by limitation, and although the present invention has been described in detail with reference to preferred arrangements, a person skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. A device for extracting titanium liquid from waste acid sludge in olefin polymerization industry is characterized in that: comprises a normal temperature and pressure hydrolysis system, an ozone catalytic oxidation system, an intermediate filtration system, an ammonia water neutralization dephosphorization desiliconization and magnesium addition system and a tubular microfiltration membrane system; the normal temperature and normal pressure hydrolysis system comprises a primary hydrolysis system and a secondary hydrolysis system; the liquid outlet end of the hydrolysate of the normal-temperature normal-pressure hydrolysis system is connected to the liquid inlet end of the ozone catalytic oxidation system through a water pump and a hydrolysis supernatant liquid output pipeline; the liquid outlet end of the ozone catalytic oxidation system is connected to the liquid inlet end of the intermediate filtering system through a pipeline; the liquid outlet end of the intermediate filtering system is connected to the liquid inlet end of the ammonia water neutralization and magnesium addition phosphorus and silicon removal system through a pipeline; the liquid outlet end of the ammonia water neutralization and magnesium addition dephosphorization and desilicification system is connected to the liquid inlet end of the tubular microfiltration membrane system through a pipeline.
2. The apparatus for extracting titanium liquid from acid sludge in olefin polymerization industry according to claim 1, wherein: the normal temperature and pressure hydrolysis system comprises a primary hydrolysis system, a secondary hydrolysis system, a waste acid residue collecting system, a filter pressing system, a hydrolysis supernatant collecting device (5), a clear water inlet pipe (6) and a waste acid residue feeding device (7);
the primary hydrolysis system comprises: a first-stage hydrolysis tank (1-1), a first-stage hydrolysis circulating pump (1-2) and a first-stage hydrolysis output pump (1-3); the secondary hydrolysis system comprises: a secondary hydrolysis tank (2-1), a secondary hydrolysis circulating pump (2-2) and a secondary hydrolysis output pump (2-3); the waste acid sludge collecting system comprises: a sludge box (3-1) and a sludge feed pump (3-2);
the primary hydrolysis tank (1-1) and the secondary hydrolysis tank (2-1) are respectively provided with a waste acid residue inlet, a waste acid residue and circulating water outlet, a liquid inlet, a hydrolysis supernatant outlet and a circulating water inlet;
a waste acid residue inlet of the primary hydrolysis tank (1-1) is connected with the waste acid residue feeding device (7); a liquid inlet of the first-stage hydrolysis tank (1-1) is connected to the clear water inlet pipe (6) through a branch pipeline, and a first-stage hydrolysis tank water inlet valve (1-4) is arranged on the branch pipeline; the waste acid sludge and circulating water outlet of the first-stage hydrolysis tank (1-1) is connected to the water inlet end of the first-stage hydrolysis circulating pump (1-2) through a pipeline, the water outlet end pipeline of the first-stage hydrolysis circulating pump (1-2) is divided into two branch pipelines which are respectively connected to the circulating water inlet of the first-stage hydrolysis tank (1-1) and the waste acid sludge inlet of the second-stage hydrolysis tank (2-1), wherein the branch pipeline connected with the circulating water inlet of the first-stage hydrolysis tank (1-1) is provided with a first-stage hydrolysis tank inlet circulating valve (1-5), and the branch pipeline connected with the waste acid sludge inlet of the second-stage hydrolysis tank (2-1) is provided with a first-stage hydrolysis pump outlet discharge valve (1-6); a supernatant outlet of the primary hydrolysis tank (1-1) is connected to a water inlet end of the primary hydrolysis output pump (1-3), and a water outlet pipeline of the primary hydrolysis output pump (1-3) is connected to a hydrolysis supernatant collecting device (5);
a liquid inlet of the secondary hydrolysis tank (2-1) is connected to the clear water inlet pipe (6) through a branch pipeline, and a water inlet valve (2-4) of the secondary hydrolysis tank is arranged on the branch pipeline; the waste acid sludge and circulating water outlet of the second-stage hydrolysis tank (2-1) is connected to the water inlet end of the second-stage hydrolysis circulating pump (2-2) through a pipeline, the water outlet end pipeline of the second-stage hydrolysis circulating pump (2-2) is divided into two branch pipelines which are respectively connected to the circulating water inlet of the second-stage hydrolysis tank (2-1) and the inlet of the sludge tank (3-1), wherein the branch pipeline connected with the circulating water inlet of the second-stage hydrolysis tank (2-1) is provided with a second-stage hydrolysis tank inlet circulating valve (2-5), and the branch pipeline connected with the inlet of the sludge tank (3-1) is provided with a second-stage hydrolysis pump outlet discharge valve (2-6); a supernatant outlet of the secondary hydrolysis tank (2-1) is connected to a water inlet end of the secondary hydrolysis outward delivery pump (2-3), and a water outlet pipeline of the secondary hydrolysis outward delivery pump (2-3) is connected to a hydrolysis supernatant collecting device (5);
an outlet of the sludge tank (3-1) is connected with a feed end of a sludge feed pump (3-2), a discharge end of the sludge feed pump (3-2) is connected to a filter pressing system through a pipeline, and a filtrate discharge pipeline of the filter pressing system is connected to the secondary hydrolysis tank (2-1).
3. The apparatus for extracting titanium liquid from acid sludge in olefin polymerization industry according to claim 1, wherein: the ozone catalytic oxidation system comprises an ozone reaction tower (8-1), an ozone generator (8-2), an ozone destructor (8-3) and an oxidation water production tank (8-4); the top of the ozone reaction tower (8-1) is provided with an ozone destructor (8-3), the inside of the ozone reaction tower (8-1) is provided with an upper layer of clapboard (8-5) with holes and a lower layer of clapboard with holes, a catalyst packing layer is arranged between the two layers of clapboards, the bottom of the ozone reaction tower (8-1) is fixed with an air duct (8-6), the air duct (8-6) is provided with a plurality of micron bubble aeration heads (8-7), and an air inlet interface of the air duct (8-6) is connected with an air duct of the ozone generator (8-2); a hydrolysis supernatant inlet (8-8) is arranged on the side wall of the ozone reaction tower (8-1) below the catalyst packing layer, and the hydrolysis supernatant inlet (8-8) is connected to a hydrolysate liquid outlet end of the normal-temperature normal-pressure hydrolysis system through a pipeline; a water outlet (8-9) after reaction is arranged on the side wall of the ozone reaction tower (8-1) above the catalyst packing layer, and the water outlet (8-9) after reaction is connected with a water inlet of the oxidation product water tank (8-4) through a pipeline;
the middle filtering system comprises a filter (9-1) and a filter water feeding pump (9-2) connected with the filter, a water outlet of the oxidation product water tank (8-4) is connected with a water inlet end of the filter water feeding pump (9-2) through a pipeline, a water outlet end of the filter water feeding pump (9-2) is connected with a water inlet end of the filter (9-1), and a water outlet end of the filter (9-1) is connected with the ammonia water neutralization and magnesium addition phosphorus and silicon removal system;
the ammonia water neutralization and magnesium adding phosphorus and silicon removal system comprises an ammonia water neutralization tank (10-1), a phosphorus and silicon removal tank (10-2) which is communicated with the ammonia water neutralization tank and has a conical bottom, a neutralization sludge discharge pump (10-3), an ammonia water feeding device and a magnesium agent feeding device, wherein a water inlet of the ammonia water neutralization tank (10-1) is connected with a water outlet end of the filter (9-1), the ammonia water neutralization tank (10-1) is connected with the phosphorus and silicon removal tank (10-2) through an overflow port, a precipitation outlet is arranged at the bottom of the phosphorus and silicon removal tank (10-2) and is connected to the neutralization sludge discharge pump (10-3) through a pipeline, a titanium hydroxide suspension overflow port is arranged on the side wall of the phosphorus and silicon removal tank (10-2), and the titanium hydroxide suspension overflow port is connected to the tubular microfiltration membrane system; the ammonia water adding device comprises an ammonia water storage tank (10-4) and an ammonia water dosing pump (10-5), wherein the liquid outlet end of the ammonia water storage tank (10-4) is connected with the liquid inlet end of the ammonia water dosing pump (10-5), and the liquid outlet end of the ammonia water dosing pump (10-5) is connected to the liquid inlet pipeline of the ammonia water neutralizing tank (10-1); the magnesium agent feeding device comprises a magnesium agent feeding box (10-6) and a magnesium agent feeding pump (10-7), wherein the liquid outlet end of the magnesium agent feeding box (10-6) is connected with the liquid inlet end of the magnesium agent feeding pump (10-7), and the liquid outlet end of the magnesium agent feeding pump (10-7) is connected to the liquid inlet pipeline of the ammonia water neutralizing box (10-1).
4. The apparatus for extracting titanium liquid from acid sludge in olefin polymerization industry according to claim 3, wherein: the tubular microfiltration membrane system comprises a tubular membrane water feeding pump (11-1), a tubular membrane circulating pump (11-2), a tubular membrane device (11-3), a tubular membrane water production tank (11-4), a neutralization water pump (11-5), a titanium hydroxide feed liquid tank (11-6), a tubular membrane cleaning device and an automatic control device; the liquid inlet end of the tubular membrane water feeding pump (11-1) is connected with a titanium hydroxide suspension overflow port of the phosphorus and silicon removing tank (10-2) through a pipeline, the liquid outlet end of the tubular membrane water feeding pump (11-1) is connected with the liquid inlet end of the tubular membrane circulating pump (11-2), the liquid outlet end of the tubular membrane circulating pump (11-2) is connected with the liquid inlet of the tubular membrane device (11-3), the concentrated liquid outlet of the tubular membrane device (11-3) is connected to the titanium hydroxide feed liquid tank (11-6) through a pipeline, a feed liquid control valve (11-10) is arranged on the pipeline between the concentrated liquid outlet of the tubular membrane device (11-3) and the titanium hydroxide feed liquid tank (11-6), and the pipeline between the feed liquid control valve (11-10) and the concentrated liquid outlet of the tubular membrane device (11-3) is communicated with the tubular membrane water feeding pump (11-1) and the tubular membrane (11-2) through a branch pipeline -2) a line between; a product water outlet of the tubular membrane device (11-3) is connected to a liquid inlet end of the tubular membrane water production tank (11-4) through a product water outlet pipeline, a product water control valve (11-11) is arranged on the product water outlet pipeline, a liquid outlet end of the tubular membrane water production tank (11-4) is connected to a liquid inlet end of a neutralization water pump (11-5), and a liquid outlet end of the neutralization water pump (11-5) is connected with a hydrochloric acid neutralization device; the automatic control device is electrically connected with the tubular membrane water feeding pump (11-1), the tubular membrane circulating pump (11-2), the neutralizing water pump (11-5) and the water pump in the tubular membrane cleaning device to control the work of each water pump.
5. The apparatus for extracting titanium liquid from acid sludge in olefin polymerization industry according to claim 4, wherein: the tubular membrane cleaning device comprises a tubular membrane backwashing pump (11-7) and a chemical cleaning device, wherein the chemical cleaning device comprises a tubular membrane cleaning water tank (11-8) and a tubular membrane cleaning pump (11-9); the liquid outlet end of the tubular membrane water production tank (11-4) is provided with a branch pipeline connected with the liquid inlet end of the tubular membrane backwashing pump (11-7), the liquid outlet end of the tubular membrane backwashing pump (11-7) is connected with the product water outlet pipeline of the tubular membrane device (11-3), and the connection point is positioned between the product water outlet of the tubular membrane device (11-3) and the product water control valve (11-11); the liquid outlet of the tubular membrane cleaning water tank (11-8) is connected with the liquid inlet end of the tubular membrane cleaning pump (11-9), the liquid outlet end of the tubular membrane cleaning pump (11-9) is connected to a liquid inlet pipeline between the tubular membrane circulating pump (11-2) and the liquid inlet of the tubular membrane device (11-3) through a pipeline, and a branch pipeline is respectively divided from the concentrated liquid outlet and the product water outlet of the tubular membrane device (11-3) and is connected to the liquid inlet of the tubular membrane cleaning water tank (11-8).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112575196A (en) * | 2020-12-24 | 2021-03-30 | 中国石油化工股份有限公司 | Method and equipment for extracting high-purity titanium liquid from olefin polymerization industrial waste acid residues |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112575196A (en) * | 2020-12-24 | 2021-03-30 | 中国石油化工股份有限公司 | Method and equipment for extracting high-purity titanium liquid from olefin polymerization industrial waste acid residues |
| CN112575196B (en) * | 2020-12-24 | 2023-11-03 | 中国石油化工股份有限公司 | Method and equipment for extracting high-purity titanium liquid from olefin polymerization industrial waste acid sludge |
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