CN107739081B - Environment-friendly treatment process for titanium tetrachloride residual feed liquid - Google Patents
Environment-friendly treatment process for titanium tetrachloride residual feed liquid Download PDFInfo
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- CN107739081B CN107739081B CN201711052837.0A CN201711052837A CN107739081B CN 107739081 B CN107739081 B CN 107739081B CN 201711052837 A CN201711052837 A CN 201711052837A CN 107739081 B CN107739081 B CN 107739081B
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses an environment-friendly treatment process of titanium tetrachloride residual feed liquid, which specifically comprises the following steps of S1: communicating the material collecting tank with the titanium tetrachloride production device, wherein the interior of the material collecting tank is in a negative pressure state, and vacuumizing the residual titanium tetrachloride material liquid into the material collecting tank; s2: the upper part of the material collecting tank is connected with a vacuum pump, and a washer is arranged between the vacuum pump and the material collecting tank; gas, smoke and liquid foam generated by volatilization of the residual titanium tetrachloride feed liquid when entering the material collecting tank enter a scrubber communicated with the material collecting tank under the suction action of a vacuum pump, are washed and purified by alkaline solution in the scrubber and are pumped and exhausted by the vacuum pump; s3: the titanium tetrachloride residual feed liquid collected in the material collecting tank is pumped to the rotary reactor through a self-priming pump; in a rotary reactor, the residual feed liquid of titanium tetrachloride and the lime powder in the reactor are subjected to intermittent controlled reaction. According to the process disclosed by the invention, the environment-friendly treatment of the titanium tetrachloride residual liquid can be realized under the conditions of no smoke and no dust.
Description
Technical Field
The invention relates to a clean and environment-friendly method for treating titanium tetrachloride residues, belonging to the technical field of chemical clean production.
Background
The chlorination process for producing titanium tetrachloride from titanium raw materials such as high titanium slag, rutile, ilmenite and the like inevitably generates liquid or liquid-solid mixed titanium tetrachloride residual waste, once the waste is discharged from a production device, the waste must be properly disposed, otherwise, the environment is polluted, and equipment is corroded.
The titanium tetrachloride residue in the invention refers to titanium tetrachloride-containing waste liquid generated by emptying, replacing and cleaning equipment pipelines of a titanium tetrachloride production device before overhauling, and titanium tetrachloride-containing waste liquid generated by cleaning equipment containers after long-term shutdown of the device. The waste liquid contains titanium tetrachloride liquid, smoke dust, titanium tetrachloride hydrolysate and the like, has complex chemical components, has the characteristics of high acidity, high corrosivity and volatility, and is extremely difficult to treat.
At present, the common method for cleaning and disposing titanium tetrachloride residue in the industry is to adopt a large amount of lime powder (main component Ca (OH))2) The materials are put into a pipeline of equipment to clean a discharge port, the discharge speed is controlled, manual mixing is carried out while discharging, the accumulated materials of the device are gradually discharged, and then mixing is continued. Ensuring the rich margin of the lime powder feeding amount, enabling the feed liquid to be in a dry and scattered small ball shape after being basically neutralized in acid, and then transferring a material pile for continuous reaction; after discharging, a large amount of water is injected into the pipeline of the equipment for replacement, and the replaced sewage is discharged from the device for additional treatment; the accumulated materials in the material mixing field are also washed clean by a large amount of water. The method for disposing the titanium tetrachloride waste is simple and extensive, the smoke on site is diffused, the smell is pungent, the dirt slag is scattered, the waste water flows transversely, the corrosion is serious, and the requirements of labor sanitation and environmental protection are not met.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide an environment-friendly treatment process of titanium tetrachloride residual feed liquid, which is characterized in that titanium tetrachloride residual feed liquid collected from a production device is rapidly mixed with a lime powder layer in a rotary reactor in batches and is subjected to controllable intermittent reaction under a severe rolling state, so that the titanium tetrachloride residual feed liquid is fully neutralized and solidified by the lime powder layer, titanium tetrachloride atomization is reduced and avoided, and the whole treatment process is highly clean and environment-friendly without smoke diffusion and dust dispersion.
In order to achieve the above purpose, the invention provides the following technical scheme:
the environment-friendly treatment process of the residual titanium tetrachloride feed liquid comprises the following steps of:
s1: communicating a material collecting tank with negative pressure inside with a titanium tetrachloride production device, and vacuumizing residual titanium tetrachloride feed liquid in the production device into the material collecting tank;
s2: the upper part of the material collecting tank is connected with a vacuum pump, and a washer is arranged between the vacuum pump and the material collecting tank; gas, smoke and liquid foam generated by volatilization of the residual titanium tetrachloride feed liquid when entering the material collecting tank enter the scrubber under the suction action of the vacuum pump, are washed and purified by alkaline solution in the scrubber and are pumped and exhausted by the vacuum pump;
s3: pumping the titanium tetrachloride residual feed liquid collected in the material collecting tank into a rotary reactor through a self-priming pump, and carrying out intermittent control reaction with a lime powder layer in the rotary reactor;
the pumping pressure (allowing the vacuum height to be sucked) of the self-sucking pump is greater than the vacuum suction force in the material collecting tank so as to overcome the vacuum of the material collecting tank and enable the material liquid to be normally conveyed to the rotary reactor.
According to the technical scheme, the residual feed liquid of titanium tetrachloride in the titanium tetrachloride production device is sucked into the material collecting tank in vacuum and stored, and the titanium tetrachloride is volatilized easily to generate gas carrying titanium tetrachloride smoke, foam and other substances when entering the material collecting tank. The volatile gas can change the negative pressure state in the material collecting tank, thereby influencing the vacuum suction effect of the residual material liquid, so the process of the invention ensures that the volatile gas flow absorbs and purifies acidic substances which can pollute the environment through alkaline solution in the scrubber under the pumping action of the vacuum pump and then is pumped and exhausted by the vacuum pump, thereby maintaining the negative pressure state in the material collecting tank, realizing the normal vacuum suction of the residual material liquid of titanium tetrachloride in the production device and simultaneously avoiding the pollution of the exhaust gas to the external environment. When a certain amount of titanium tetrachloride residual feed liquid in the material collecting tank is collected, a self-priming pump is started, the titanium tetrachloride residual feed liquid in the material collecting tank is pumped into a rotary reactor in batches, and is fully mixed with a lime powder layer in the reactor in a violent rolling state, and intermittent control reaction is carried out, so that the titanium tetrachloride residual feed liquid is ensured to fully react with the lime powder, and is prevented from being discharged out of equipment after being reacted and atomized with water in the air, and serious pollution to the environment is caused.
Further, the intermittent control reaction is mainly realized by intermittent forward and reverse operation of a rotary reactor: when the rotary reactor rotates forwards, the self-sucking pump conveys the residual titanium tetrachloride feed liquid in the material collecting tank into the rotary reactor to react with a lime powder layer which is placed in the rotary reactor in advance; wherein, the conveying speed of the titanium tetrachloride residual feed liquid is controlled, the PH value of a mixed reaction material layer of titanium tetrachloride residual liquid and lime powder in the rotary reactor is controlled within a range of more than or equal to 8, the reaction temperature does not exceed 90 ℃, the conveying of the titanium tetrachloride residual feed liquid is stopped when the PH value of the material layer is gradually reduced to a range of 8.0-8.5, maintaining the rotary reactor to rotate forwards for 3-5min, and then rotating backwards to discharge the treated waste solid material from the discharge hole, then the lime powder is added again by corotation, after the lime powder layer in the reactor reaches a certain thickness, the self-priming pump is restarted to pump a proper amount of titanium tetrachloride residual feed liquid into the rotary reactor, and then repeating the process steps to realize intermittent control treatment on the titanium tetrachloride residual feed liquid, ensuring the surplus state of the lime powder in the treatment process and effectively preventing the titanium tetrachloride from being atomized and diffused to cause environmental pollution.
Further, the intermittent control reaction in step S3 is a circulation step mainly including the following steps:
s30: loading a predetermined amount of lime powder into the rotary reactor in the forward rotation process of the rotary reactor to form a lime powder layer;
s31: starting a self-sucking pump, and conveying the residual titanium tetrachloride feed liquid in the material collecting tank into a rotary reactor to react with lime powder;
s32: when the PH value of the lime powder layer reaches 8.0-8.5, stopping conveying the residual titanium tetrachloride feed liquid, and maintaining the rotary reactor to rotate positively for 3-5 min;
s33: after the full reaction of S32, the rotary reactor is reversed to discharge the reacted waste solid material.
Furthermore, the equipment used in the process also comprises a sanitary exhaust fan, and the waste gas in the rotary reactor is exhausted by the sanitary fan, and the rotating speed of the sanitary fan is adjusted to control the exhaust volume so as to prevent the smoke in the rotary reactor from overflowing.
Further, the lime powder is hydrated lime or active hydrated lime powder, the active hydrated lime powder is obtained by high-temperature digestion of quicklime at the temperature of more than 100 ℃, and the active hydrated lime powder does not contain lumps with the diameter of more than 20 mm.
The inventor verifies through a plurality of experiments that the active hydrated lime powder which is obtained by slaking quicklime at high temperature of more than 100 ℃ and does not contain lumps of more than 20mm is preferably used as a reaction raw material, and the fine active hydrated lime can be in more uniform and sufficient contact with the residual titanium tetrachloride feed liquid, so that the fast and sufficient neutralization and solidification of the feed liquid participating in the titanium tetrachloride can be realized, the atomization of the titanium tetrachloride and the moisture in the air is prevented, and the environment pollution caused by the overflow of the titanium tetrachloride and the moisture in the air is effectively prevented.
Furthermore, the free water content in the active hydrated lime powder is controlled within 5-20%, and preferably, the free water content is 5-10%.
The main chemical reaction of titanium tetrachloride residue and hydrated lime powder is as follows:
TiCl4+ Ca（OH）2+ H2O→ CaCl2•nH2O + TiO2
TiOHCl3•4H2O + Ca（OH）2+ H2O → CaCl2•nH2O + TiO2
HCl + Ca（OH）2+ H2O → CaCl2•nH2O
reaction principle and experimental research show that the slaked lime powder has good dispersibility and reactivity when the water content is 5-20%; too high a water content leads to a decrease in the dispersibility of the reaction bed, resulting in TiCl4The preferential reaction with free water generates a large amount of smoke, which is easy to cause environmental pollution; when the water content is below 5%, the lime powder is easy to scatter dust, and the reaction activity is reduced; when the water content of the hydrated lime is 5-10%, the hydrated lime and titanium tetrachloride are remainedThe reaction effect of the feed liquid is optimal.
Further, the alkaline solution in step S2 is sodium hydroxide solution with a concentration of 5-30% by weight.
Further, in the step S31, the self-priming pump conveys the residual titanium tetrachloride feed liquid to a position 50-150mm inside the lime powder layer through a conveying pipe. Preferably, a small tube with the inner diameter of 10-30 mm is used in the loosening process of the self-sucking pump.
The titanium tetrachloride residual material is conveyed by the conveying small pipes, so that the area of a feed inlet of the titanium tetrachloride residual material can be effectively controlled in a small range, the sufficient reaction between the titanium tetrachloride residual material liquid and the lime powder layer is further ensured, and the titanium tetrachloride material liquid is prevented from being atomized and diffused. The insertion depth of the conveying small pipe is that the position where the materials on the middle upper part of the material layer in the rotary roller are actively turned over is preferably inserted into the position 50-150mm inside the lime powder layer, so that the problem that the titanium tetrachloride material liquid is easy to directly contact with air to be atomized due to too shallow insertion or the small pipe is easy to block due to too deep insertion can be effectively avoided.
Further, the conveying speed of the titanium tetrachloride residual feed liquid in the step S31 is controlled to ensure that the pH value of a lime powder layer in the rotary reactor is more than or equal to 8, so that the lime powder layer is ensured to keep an alkaline active state capable of neutralizing and curing the titanium tetrachloride feed liquid, and the excessive pollution caused by the fact that the titanium tetrachloride residual feed liquid cannot be neutralized and cured by surplus active calcium hydroxide is avoided.
Meanwhile, the reaction speed is controlled to control the reaction temperature in the mixture layer within 90 ℃, so that the high-temperature gasification of titanium tetrachloride caused by overhigh temperature is avoided from escaping from equipment, the environmental pollution is avoided, and the influence on the reaction speed and the treatment efficiency caused by overlow temperature is avoided.
Furthermore, in the equipment used in the process, the vacuum material suction device is connected with a discharge port of a pipeline of titanium tetrachloride production equipment through a hose or a soft rubber pipe is directly extended into a material accumulation position in the container; the connection mode is socket joint connection or flange connection. Preferably, the vacuum material suction device adopts a movable vacuum material suction device, is provided with a movable auxiliary mechanism, and can be conveniently transferred and applied to different parts of a titanium tetrachloride production line.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the environment-friendly treatment process of the titanium tetrachloride residual feed liquid, provided by the invention, while the titanium tetrachloride residual feed liquid in the production device is collected by vacuum suction, the collected titanium tetrachloride residual feed liquid is pumped into the rotary reactor in batches through the self-sucking pump to perform intermittent control reaction with the lime powder layer, so that the titanium tetrachloride residual feed liquid is fully neutralized by the lime powder layer, is converted into I-type waste solid materials and is discharged. The whole residual material treatment process can realize high cleanness and environmental protection without smog diffusion and dust dispersion.
2. By combining the process matching equipment, the invention further realizes full-automatic or semi-automatic treatment process of the titanium tetrachloride residual feed liquid, and greatly reduces the labor cost.
3. According to the treatment process disclosed by the invention, substances in the titanium tetrachloride residual feed liquid can be fully converted into I-type waste solid materials and used for building materials or landfill treatment, so that the environmental friendliness of products obtained after the titanium tetrachloride residual feed liquid is treated is further improved.
Description of the drawings:
FIG. 1 is a schematic diagram of the equipment used in the process of the present invention.
The labels in the figure are: 1-TiCl4The method comprises the following steps of (1) discharging a residue, 2-collecting tank, 3-self-sucking pump, 4-scrubber, 5-vacuum pump, 6-rotary reactor, 7-sanitary fan, 8-lime powder feeding port, 9-waste solid material discharging port, A-TiCl4Production equipment, B-alkaline solution and C-waste gas are emptied.
Detailed Description
The invention will be described in further detail with reference to the accompanying apparatus and embodiments of the process of the invention as shown in figure 1. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention.
As shown in figure 1, the equipment adopted by the process of the invention specifically comprises three major parts, namely a vacuum material suction device, a washer and a rotary reactor, wherein the vacuum material suction deviceComprising reacting with TiCl4The material collecting tank (2) is communicated with the residue discharge port (1), and the vacuum pump (5) and the self-sucking pump (3) are respectively communicated with the upper part of the material collecting tank (2) and the lower part of the material collecting tank (2); the washer (4) is connected between the vacuum pump (5) and the material collecting tank (2); the lower part of the material collecting tank (2) is communicated with a self-sucking pump (3), and the other end of the self-sucking pump (3) is communicated with a rotary reactor (6); the rotary reactor (6) is a horizontal rotary cylinder, the two ends of the horizontal rotary cylinder are provided with an air draft cover and an air draft pipe, the air draft cover at one end is provided with a feeding hole communicated with a self-priming pump, and the air draft cover at the other end is fixed with a lime powder feeding hole (8) and a waste solid material discharging hole (9) after reaction treatment. The sanitary fan (7) is respectively communicated with the outlet of the vacuum pump and the exhaust pipes at the two ends of the rotary cylinder and is used for exhausting waste gas.
Example 1
By combining the equipment, the environment-friendly treatment process for the titanium tetrachloride residual feed liquid comprises the following specific operation steps:
1) a discharge port (1) for connecting the vacuum material sucking device and the production device; sodium hydroxide solution with the weight percentage concentration of 5% -30% is contained in the washer (4); starting a sanitary fan (7);
2) before the pumping of the residual liquid is started, a rotary reactor (6) is started, the rotary reactor (6) rotates forwards at a proper speed, and a proper amount of active hydrated lime with the free water content of 5 percent is added from a lime powder feeding hole (8); the active slaked lime powder is obtained by high-temperature slaking quicklime at 100 deg.C or higher and does not contain lumps of 20mm or more.
3) After the lime powder loading capacity in the rotary reactor (6) reaches the rated loading capacity and a lime powder material layer with a certain thickness is formed, starting a vacuum pump (5) and opening a discharge valve to ensure that residual titanium tetrachloride feed liquid in the production device (A) is sucked into the material collecting tank in a vacuum manner when the interior of the material collecting tank (2) reaches a negative pressure state;
4) inserting a titanium tetrachloride conveying small pipe connected with a self-sucking pump and a rotary reactor into the active hydrated lime powder layer at a position of 50-150mm, and starting the self-sucking pump (3) to slowly input titanium tetrachloride residue into the rotary reactor (6). The rotating speed of the self-sucking pump (3) is adjusted to control the reaction temperature of the reaction material layer within 90 ℃, and the PH value of the material bed is kept within the range of PH being more than or equal to 8, so that the smoke is prevented from occurring.
5) When the PH value of the lime powder layer in the rotary reactor is within the range of 8.0-8.5, the self-priming pump (3) is closed, the residual titanium tetrachloride liquid is stopped being conveyed into the rotary reactor (6), and the rotary reactor (6) is kept rotating positively for 3-5 min.
6) Thereafter, the rotary reactor (6) is reversed to remove the waste solids.
7) Repeating the steps 2) to 6) until the titanium tetrachloride residual liquid in the production device is completely treated.
Wherein, the air draft of the rotary reactor (6) is conveyed and emptied by a sanitary fan (7). The rotating speed of the fan is adjusted to control the air pumping quantity, so that the smoke of the rotary reactor is not overflowed.
Example 2
The same process steps and process parameters were used as in example 1, except that the free water content of the active slaked lime powder in 2) was changed to 10%.
Example 3
The same process steps and process parameters were used as in example 1, except that the free water content of the active slaked lime powder in 2) was changed to 15%.
Example 4
The same process steps and process parameters as in example 1 were used except that the free water content of the active hydrated lime powder in 2) was changed to 20%.
The experimental results of the four examples show that in the process of neutralizing the titanium tetrachloride residual liquid in the examples, no obvious titanium tetrachloride smoke or liquid foam is entrained in the waste gas discharged from the sanitary fan, and the waste solid slag discharged from the rotary reactor finally reaches the I-type general industrial solid waste standard. Therefore, according to the titanium tetrachloride residual feed liquid treatment process and parameters in the embodiments 1 to 4 of the invention, the titanium tetrachloride residual feed liquid can be ensured to be fully neutralized and solidified with lime powder in the rotary reactor, the condition that the environment is polluted due to gas overflow caused by atomization and gasification of titanium tetrachloride is effectively avoided, and the high cleanness and environmental protection without smoke diffusion and dust dispersion can be practically realized in the whole residual material treatment process.
Comparative example 1
The influence of the reaction temperature of the mixed reaction material layer in the rotary reactor on the treatment effect of the residual titanium tetrachloride feed liquid is verified by arranging a corresponding comparative example.
Comparative example 1-1 neutralization treatment of the residual titanium tetrachloride feed liquid was carried out by the same process and parameters as in example 1 except that the feeding speed of the residual titanium tetrachloride feed liquid to the rotary reactor in step 4) was adjusted so that the reaction temperature in the mixed reaction layer reached 110 ℃.
Comparative examples 1-2 neutralization treatment of the residual titanium tetrachloride feed liquid was carried out by the same process and parameters as in example 1 except that the feeding speed of the residual titanium tetrachloride feed liquid to the rotary reactor in step 4) was adjusted so that the reaction temperature in the mixed reaction layer reached 70 ℃.
It was found that, in comparison with example 1, during the neutralization treatment of the titanium tetrachloride residual liquid according to the process conditions in comparative example 1-1, a large amount of titanium tetrachloride fumes and liquid foams were significantly entrained in the exhaust gas sucked and discharged from the sanitary fan. No obvious titanium tetrachloride smog or liquid foam is discharged from a sanitary ventilator in the process of neutralizing the titanium tetrachloride residual feed liquid according to the process conditions in the comparative examples 1-2, but the time for treating the same amount of titanium tetrachloride residual feed liquid is longer in the comparative examples 1-2, and the operation efficiency is relatively lower.
Comparative example 2
And the influence of the size of the used lime powder on the treatment effect of the residual titanium tetrachloride feed liquid is verified by setting a corresponding comparison example.
Comparative example 2-1 neutralization treatment of titanium tetrachloride residual feed liquid was carried out by the same process and parameters as in example 1 except that the active slaked lime powder in step 2) was changed to slaked lime powder containing lumps having a diameter of 30mm or more.
Compared with example 1, the detection shows that in the process of neutralizing the titanium tetrachloride residual feed liquid by using the active hydrated lime powder with the diameter of more than 30mm in the proportion 2-1, a large amount of obvious titanium tetrachloride smoke and liquid foam are carried in the waste gas sucked and discharged from the sanitary fan.
Comparative example 3
And verifying the influence of the pH value of a mixed reaction material layer in the rotary reactor on the treatment effect of the titanium tetrachloride residual feed liquid when the titanium tetrachloride residual feed liquid is stopped being conveyed into the rotary reactor by arranging a corresponding comparative example.
Comparative example 3-1 neutralization treatment of titanium tetrachloride residual feed liquid was carried out by the same process and parameters as in example 1 except for changing the step 5) to: when the PH value of the lime powder layer in the rotary reactor is within the range of 8.6-9.5, the self-priming pump (3) is closed, the residual titanium tetrachloride liquid is stopped being conveyed into the rotary reactor (6), and the rotary reactor (6) is kept rotating positively for 3-5 min. .
Comparative examples 3-2 neutralization treatment of titanium tetrachloride residual feed liquid was carried out by the same process and parameters as in example 1 except for changing the step 5) to: and when the PH value of the lime powder layer in the rotary reactor is within the range of 7-7.9, closing the self-sucking pump (3), stopping conveying the residual titanium tetrachloride liquid into the rotary reactor (6), and keeping the rotary reactor (6) rotating positively for 3-5 min.
According to the detection, compared with the example 1, in the process of neutralizing the titanium tetrachloride residual liquid by the comparative examples 3-1 and 3-2, a large amount of obvious titanium tetrachloride smoke and liquid foam are carried in the waste gas sucked and discharged from the sanitary fan.
Comparative example 4
And the influence of the free water content in the active hydrated lime powder on the treatment effect of the residual titanium tetrachloride feed liquid is verified by setting a corresponding comparative example.
Comparative example 4-1 neutralization treatment of titanium tetrachloride residual feed liquid was carried out by the same process and parameters as in example 1 except that the free water content of active hydrated lime powder in step 2) was adjusted to 3%.
Comparative examples 4-2 neutralization treatment of the residual feed liquid of titanium tetrachloride was carried out by the same process and parameters as in example 1 except that the free water content of active hydrated lime powder in step 2) was adjusted to 30%.
As a result of detection, compared with example 1, in the process of neutralizing the titanium tetrachloride residual feed liquid according to the process conditions in comparative example 4-1, lime powder dust is entrained in the exhaust gas sucked and discharged from the sanitary fan, the reaction speed is slow, and the reaction activity is reduced. In the process of neutralizing the titanium tetrachloride residual feed liquid according to the process conditions in the comparative example 4-2, the dispersibility of the lime powder layer is reduced, the lime powder layer is not uniformly mixed with the titanium tetrachloride residual feed liquid, and a large amount of obvious titanium tetrachloride smoke or liquid foam is discharged from the sanitary air draft machine.
Claims (7)
1. An environment-friendly treatment process of titanium tetrachloride residual feed liquid is characterized in that equipment used by the process comprises a vacuum material suction device, a rotary reactor and a sanitary fan, wherein the vacuum material suction device comprises a material collecting tank, a washer, a vacuum pump and a self-sucking pump; the specific operation of the process comprises the following steps:
s1: communicating a material collecting tank with negative pressure inside with a titanium tetrachloride production device, and vacuumizing residual titanium tetrachloride feed liquid in the production device into the material collecting tank;
s2: the upper part of the material collecting tank is connected with a vacuum pump, and a washer is arranged between the vacuum pump and the material collecting tank; gas, smoke and liquid foam generated by volatilization of the residual titanium tetrachloride feed liquid when entering the material collecting tank enter the scrubber under the suction action of the vacuum pump, are washed and purified by alkaline solution in the scrubber and are pumped and exhausted by the vacuum pump;
s3: the titanium tetrachloride residual feed liquid collected in the material collecting tank is pumped into a rotary reactor through a self-priming pump and performs intermittent control reaction with a lime powder layer in the rotary reactor; wherein the content of the first and second substances,
the pumping pressure of the self-sucking pump allows the sucking vacuum height to be larger than the vacuum suction force in the material collecting tank;
the lime powder is active hydrated lime powder, and the active hydrated lime powder does not contain lumps of more than 20 mm;
the free water content of the lime powder is 5-20%;
the self-priming pump conveys the residual titanium tetrachloride feed liquid to a position 50-150mm inside the lime powder layer through a conveying pipe, and a small pipe is used in the conveying process of the self-priming pump, and the inner diameter of the small pipe is phi 10-phi 30 mm.
2. The environment-friendly treatment process of titanium tetrachloride residual feed liquid according to claim 1, characterized in that,
the intermittent control reaction is mainly realized through intermittent forward and reverse operation of a rotary reactor, when the rotary reactor rotates forwards, a self-sucking pump conveys residual titanium tetrachloride feed liquid in an aggregate tank into the rotary reactor, and the residual titanium tetrachloride feed liquid reacts with a lime powder layer which is placed in the rotary reactor in advance; after the residual feed liquid of the titanium tetrachloride is stopped being conveyed, the rotary reactor is kept rotating positively for 3-5min, and then the rotary reactor is rotated reversely to discharge the treated waste solid material from the discharge hole, and then the lime powder is added again.
3. The environment-friendly treatment process of titanium tetrachloride residual feed liquid according to claim 1, wherein the intermittent control reaction in the step S3 mainly comprises the following steps of:
s30: loading a predetermined amount of lime powder into the rotary reactor in the forward rotation process of the rotary reactor to form a lime powder layer;
s31: starting a self-sucking pump, and conveying the residual titanium tetrachloride feed liquid in the material collecting tank into a rotary reactor to react with lime powder;
s32: when the PH of the mixed material liquid reaches 8.0-8.5, stopping conveying the residual material liquid of titanium tetrachloride, and maintaining the rotary reactor to rotate positively for 3-5 min;
s33: after the full reaction of S32, the rotary reactor is reversed to discharge the reacted waste solid material.
4. The environment-friendly treatment process of the titanium tetrachloride residual feed liquid as claimed in claim 1 or 3, wherein the waste gas in the rotary reactor is exhausted by a sanitary fan, and the rotation speed of the sanitary fan is adjusted to control the exhaust volume so that the smoke in the rotary reactor does not overflow.
5. The process of claim 1, wherein the alkaline solution in S2 is a sodium hydroxide solution with a concentration of 5-30% by weight.
6. The process of claim 1, wherein the feeding speed of the titanium tetrachloride residual feed liquid in S3 is controlled, and the reaction temperature is controlled within 90 ℃.
7. The environment-friendly treatment process of titanium tetrachloride residual feed liquid according to claim 1, characterized in that the equipment used in the process comprises: the vacuum material suction device is connected with a discharge port of a pipeline of titanium tetrachloride production equipment through a hose or a soft rubber pipe is directly stretched into a material accumulation position in the container; the connection mode is socket joint connection or flange connection.
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|---|---|---|---|---|
| CN101216246A (en) * | 2008-01-16 | 2008-07-09 | 西安近代化学研究所 | Revolving furnace |
| CN102173497A (en) * | 2010-12-24 | 2011-09-07 | 天津合佳威立雅环境服务有限公司 | Process of treating hazardous waste and waste acid capable of violently reacting with water |
| CN103447283A (en) * | 2013-08-30 | 2013-12-18 | 漯河兴茂钛业股份有限公司 | Safe disposal method for waste residue produced by production of titanium tetrachloride by using titanium dioxide by chlorination process |
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| CN103771735B (en) * | 2012-10-19 | 2016-03-30 | 中国石油化工股份有限公司 | White lime process polyolefin catalyst titanium-containing waste residues is utilized to prepare the method for cement |
| CN103769406B (en) * | 2012-10-19 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of processing method of polyolefin catalyst titanium-containing waste residues |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101216246A (en) * | 2008-01-16 | 2008-07-09 | 西安近代化学研究所 | Revolving furnace |
| CN102173497A (en) * | 2010-12-24 | 2011-09-07 | 天津合佳威立雅环境服务有限公司 | Process of treating hazardous waste and waste acid capable of violently reacting with water |
| CN103447283A (en) * | 2013-08-30 | 2013-12-18 | 漯河兴茂钛业股份有限公司 | Safe disposal method for waste residue produced by production of titanium tetrachloride by using titanium dioxide by chlorination process |
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