CN107673404A - The method that excessive chlorine recycles in low temperature chlorination reaction - Google Patents
The method that excessive chlorine recycles in low temperature chlorination reaction Download PDFInfo
- Publication number
- CN107673404A CN107673404A CN201711009947.9A CN201711009947A CN107673404A CN 107673404 A CN107673404 A CN 107673404A CN 201711009947 A CN201711009947 A CN 201711009947A CN 107673404 A CN107673404 A CN 107673404A
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- China
- Prior art keywords
- chlorine
- chlorination reaction
- low temperature
- excessive
- excessive chlorine
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
Abstract
Disclosed by the invention is the method that excessive chlorine recycles during a kind of low temperature chlorination of chloridization process technical field reacts, and is comprised the following steps:The chlorine that will be greater than standard proportioning first is passed through progress low temperature chlorination reaction producing titanium tetrachloride t 5 bx mixed flue gas in the chlorination reaction bed of material, then mixed flue gas made from collecting, and dedusting and condensation process are carried out to it, excessive chlorine is obtained, the part or all of excessive chlorine importing chlorination reaction bed of material is finally extracted and is recycled.The beneficial effects of the invention are as follows:This method provides condition for the excessive chloridization process design of chlorine, can reduce the alkali lye consumption that excessive chlorine processing is brought, while realizes that excessive chlorine recycles, while also has and improve TiCl4Product collection efficiency, alleviate low temperature chlorination reaction severe degree and be advantageous to the advantages that low temperature chlorination stove thermal balance is established.
Description
Technical field
Recycled the present invention relates to excessive chlorine in chloridization process technical field, more particularly to a kind of reaction of low temperature chlorination
Method.
Background technology
At present, low temperature chlorination reaction is the reaction of chlorine deficiency, and TiC reaction conversion ratios are difficult to obtain into one in its carbide slag
Step lifting.In general chemical industry application process, two kinds of substance reactions, to make one of which reaction-ure conversion-age as high as possible, often
Excessively realized by another reactant, for existing chlorination process, if taking the excessive mode of chlorine to lift mesh
Mark the conversion ratio of chloride, then chlorine excessively can then increase the chlorine consuming cost of unit product, while excessive chlorine needs
Absorption processing is carried out with alkali lye and causes the increase of unit product alkali lye consumption.
Therefore, it is necessary to develop a kind of method that excessive chlorine recycles in chlorination reaction, reaching chlorine allows excessive, energy
TiC conversion ratios in carbide slag are lifted, the purpose without increasing the consumption of unit product chlorine and alkali lye consumption.
The content of the invention
To overcome the problems such as TiC conversion ratios are not high in chlorine deficiency, carbide slag in existing low temperature chlorination reaction, institute of the present invention
Technical problems to be solved are:There is provided it is a kind of using excessive chlorine carry out low temperature chlorination reaction and make excessive chlorine recycle
Production method.
The technical solution adopted for the present invention to solve the technical problems is:
The method that excessive chlorine recycles in low temperature chlorination reaction, will be greater than the chlorine of standard proportioning first, to be passed through chlorination anti-
Answer and low temperature chlorination reaction producing titanium tetrachloride t 5 bx mixed flue gas, then mixed flue gas made from collection, and entering to it are carried out in the bed of material
Row dedusting and condensation process, obtain excessive chlorine, finally extract part or all of excessive chlorine and import the progress of the chlorination reaction bed of material
Recycle.
It is further to need to ensure the amount of chlorine being passed through in the chlorination reaction bed of material during the recycling of excessive chlorine
The 10%~200% of the proportioning that is above standard.
It is -30~25 DEG C by the temperature of dedusting and the mixed flue gas of condensation process to be further.
It is further, before excessive chlorine is imported into the chlorination reaction bed of material, first by it with entering chlorination reaction material at first
The chlorine of layer imports again after being mixed.
It is further that for the chlorination reaction bed of material including multiple, excessive chlorine can import any one chlorination reaction
The bed of material.
The beneficial effects of the invention are as follows:
1st, condition is provided for the excessive chloridization process design of chlorine, the alkali lye that excessive chlorine processing is brought can be reduced and disappeared
Consumption, while realize that excessive chlorine recycles;
2nd, TiCl is improved4Product collection efficiency, TiCl is included in excessive chlorine4Product gas, what excessive chlorine recycled
It also will not collect complete TiCl simultaneously4Product return system regathers, and improves TiCl4Product collection efficiency, reduction are not collected
TiCl4Processing cost;
3rd, stove chlorine gas concentration can be diluted into, alleviates low temperature chlorination reaction severe degree, reduce causes office because reacting acutely
The situation of portion's caking at high temperature;
4th, excessive chlorine can take away reaction surplus heat, and adjustment low temperature chlorination reaction thermal balance, excessive chlorine is that flue gas is cold
Gaseous mixture after solidifying, temperature are -30~25 DEG C, can take away reaction surplus heat after entering stove, be advantageous to low temperature chlorination stove thermal balance
Establish.
Brief description of the drawings
Fig. 1 is the theory diagram of the present invention.
Fig. 2 is another program theory diagram of the present invention.
Embodiment
The present invention is further described below in conjunction with the accompanying drawings.
The method that excessive chlorine recycles in low temperature chlorination reaction, will be greater than the chlorine of standard proportioning first, to be passed through chlorination anti-
Answer and low temperature chlorination reaction producing titanium tetrachloride t 5 bx mixed flue gas, then mixed flue gas made from collection, and entering to it are carried out in the bed of material
Row dedusting and condensation process, obtain excessive chlorine, finally extract part or all of excessive chlorine and import the progress of the chlorination reaction bed of material
Recycle, finally give circulation block diagram as shown in Figure 1.
Low temperature chlorination reaction of the prior art is typically matched using standard in order to reduce chlorine dosage, causes carbide slag
Middle TiC reaction conversion ratios are relatively low.Conversion ratio of the invention then that TiC is improved by the way of excessive chlorine is passed through, then to anti-
The mixed flue gas that should be obtained carries out reclaiming dedusting and condensation, is finally reused again, that is, improves production efficiency and quality,
It turn avoid the alkali lye consumption that processing excessive chlorine is brought.Also have simultaneously and improve TiCl4Product collection efficiency, alleviate low temperature chlorine
Change reaction severe degree and be advantageous to the advantages that low temperature chlorination stove thermal balance is established.
In order to ensure the conversion ratio of low temperature chlorination reaction, guarantee is needed to be passed through chlorination during the recycling of excessive chlorine
Amount of chlorine in the reaction bed of material is above standard the 10%~200% of proportioning.It can be entered in practical operation by valve and flowmeter
Row regulation, optimal case is to automatically adjust chlorine flowrate using automatic control system.
It is condensed mixed flue gas by the excessive chlorine of dedusting and condensation process, its composition includes Cl2、TiCl4、
CO2、CO、N2、O2According to chlorination reaction bed of material actual temperature demand -30~25 DEG C are can be controlled in Deng, condensed temperature, it is excessive
Chlorine, which enters to take away in the chlorination reaction bed of material after stove, reacts surplus heat, is advantageous to the foundation of low temperature chlorination stove thermal balance.
In order to avoid temperature inequality causes to react uneven in the chlorination reaction bed of material, the situation of localized hyperthermia's caking is caused,
Before excessive chlorine is imported into the chlorination reaction bed of material, first it is dropped with entering at first after the chlorine of the chlorination reaction bed of material is mixed
Wen Houzai is imported.
Further, as shown in Fig. 2 the chlorination reaction bed of material is including multiple, excessive chlorine can import any one
The chlorination reaction bed of material.Material in multiple chlorination reaction bed of materials can be similar and different, and lead-in mode can use uniform
Scattered mode, the temperature of condensation can be so made full use of to keep chlorination furnace thermal balance;One main reaction material can also be set
Layer, multiple small side reaction bed of materials, the excessive chlorine of recovery can import each side reaction bed of material, can so ensure main reaction material
The efficient stable of layer, and and can plays a part of recycling to excessive chlorine.
The method applied in the present invention, although its principle is similar with common resource recycling, for low temperature chlorination
For reaction process, this method provides condition for the excessive chloridization process design of chlorine, and with raising TiCl4Product is received
Collection efficiency, alleviate low temperature chlorination reaction severe degree and be advantageous to the advantages that low temperature chlorination stove thermal balance is established, have fine
Practicality and application prospect.
Claims (5)
1. the method that excessive chlorine recycles in low temperature chlorination reaction, it is characterized in that:The chlorine that will be greater than standard proportioning first leads to
Enter to carry out low temperature chlorination reaction producing titanium tetrachloride t 5 bx mixed flue gas in the chlorination reaction bed of material, then mixed flue gas made from collection,
And dedusting and condensation process are carried out to it, excessive chlorine is obtained, part or all of excessive chlorine is finally extracted and imports chlorination reaction
The bed of material is recycled.
2. the method that excessive chlorine recycles in low temperature chlorination reaction as claimed in claim 1, it is characterized in that:In excessive chlorine
Recycle during need to ensure that the amount of chlorine that is passed through in the chlorination reaction bed of material is above standard the 10%~200% of proportioning.
3. the method that excessive chlorine recycles in low temperature chlorination reaction as claimed in claim 1, it is characterized in that:By dedusting and
The temperature of the mixed flue gas of condensation process is -30~25 DEG C.
4. the method that excessive chlorine recycles in low temperature chlorination reaction as claimed in claim 3, it is characterized in that:By excess chlorine
Before conductance enters the chlorination reaction bed of material, first it is imported again with entering at first after the chlorine of the chlorination reaction bed of material is mixed.
5. the method that excessive chlorine recycles in low temperature chlorination reaction as claimed in claim 4, it is characterized in that:The chlorination is anti-
The bed of material is answered to include multiple, excessive chlorine can import any one chlorination reaction bed of material.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108993188A (en) * | 2018-09-26 | 2018-12-14 | 浙江凯色丽科技发展有限公司 | Environment-friendly type titanium liquid dilution device |
CN112707440A (en) * | 2019-10-25 | 2021-04-27 | 中国科学院过程工程研究所 | Method for producing titanium dioxide by low-temperature chlorination of titanium-rich material |
CN113184900A (en) * | 2021-05-12 | 2021-07-30 | 攀钢集团钒钛资源股份有限公司 | Titanium tetrachloride production method and system and raw material ratio adjusting method |
CN113651355A (en) * | 2021-09-13 | 2021-11-16 | 攀钢集团钒钛资源股份有限公司 | Titanium dioxide production system and method for distributing chlorine |
CN114956021A (en) * | 2021-11-22 | 2022-08-30 | 上海绿麟达新材料科技有限公司 | Preparation method of phosphorus pentachloride |
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CN1033264A (en) * | 1987-10-27 | 1989-06-07 | 冶金工业部攀枝花钢铁公司钢铁研究院 | The method of preparing titanic chloride using carbon-containing slag |
CN101016167A (en) * | 2006-02-09 | 2007-08-15 | 朱作远 | Process of preparing high-purity TiCl4 by preheating chlorine gas low-temperature chlorination method |
CN101164895A (en) * | 2007-10-08 | 2008-04-23 | 清华大学 | Chlorination method for producing titanium tetrachloride at low temperature |
CN102743945A (en) * | 2012-07-04 | 2012-10-24 | 金川集团股份有限公司 | Treating process for furnace gas of chlorination furnace used for production of titanium tetrachloride |
CN104619646A (en) * | 2013-03-06 | 2015-05-13 | 东邦钛株式会社 | Titanium-tetrachloride manufacturing method |
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- 2017-10-25 CN CN201711009947.9A patent/CN107673404A/en active Pending
Patent Citations (5)
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CN1033264A (en) * | 1987-10-27 | 1989-06-07 | 冶金工业部攀枝花钢铁公司钢铁研究院 | The method of preparing titanic chloride using carbon-containing slag |
CN101016167A (en) * | 2006-02-09 | 2007-08-15 | 朱作远 | Process of preparing high-purity TiCl4 by preheating chlorine gas low-temperature chlorination method |
CN101164895A (en) * | 2007-10-08 | 2008-04-23 | 清华大学 | Chlorination method for producing titanium tetrachloride at low temperature |
CN102743945A (en) * | 2012-07-04 | 2012-10-24 | 金川集团股份有限公司 | Treating process for furnace gas of chlorination furnace used for production of titanium tetrachloride |
CN104619646A (en) * | 2013-03-06 | 2015-05-13 | 东邦钛株式会社 | Titanium-tetrachloride manufacturing method |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108993188A (en) * | 2018-09-26 | 2018-12-14 | 浙江凯色丽科技发展有限公司 | Environment-friendly type titanium liquid dilution device |
CN112707440A (en) * | 2019-10-25 | 2021-04-27 | 中国科学院过程工程研究所 | Method for producing titanium dioxide by low-temperature chlorination of titanium-rich material |
CN113184900A (en) * | 2021-05-12 | 2021-07-30 | 攀钢集团钒钛资源股份有限公司 | Titanium tetrachloride production method and system and raw material ratio adjusting method |
CN113651355A (en) * | 2021-09-13 | 2021-11-16 | 攀钢集团钒钛资源股份有限公司 | Titanium dioxide production system and method for distributing chlorine |
CN113651355B (en) * | 2021-09-13 | 2023-01-24 | 攀钢集团钒钛资源股份有限公司 | Titanium dioxide production system and method for distributing chlorine |
CN114956021A (en) * | 2021-11-22 | 2022-08-30 | 上海绿麟达新材料科技有限公司 | Preparation method of phosphorus pentachloride |
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Application publication date: 20180209 |