CN110054217A - Crude titanic chloride quickly removes vanadium compounding organic matter and preparation method thereof - Google Patents
Crude titanic chloride quickly removes vanadium compounding organic matter and preparation method thereof Download PDFInfo
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- CN110054217A CN110054217A CN201910352268.4A CN201910352268A CN110054217A CN 110054217 A CN110054217 A CN 110054217A CN 201910352268 A CN201910352268 A CN 201910352268A CN 110054217 A CN110054217 A CN 110054217A
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- vanadium
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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
- C01G23/024—Purification of tetrachloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention belongs to quickly remove vanadium compounding organic matter and preparation method thereof, including synthetic base oil, aromatic naphtha, naphthenic oil, organic phosphorus compound and alkylnaphthalene except vanadium reagents field more particularly to a kind of crude titanic chloride;The synthetic base oil, aromatic naphtha, naphthenic oil, organic phosphorus compound and alkylnaphthalene mass ratio successively are as follows: 40~70:2~10:20~30:2~10:5~10.The synthetic base oil is C18~C20Alpha-olefin oligomer;The aromatic naphtha is 2# aromatic naphtha;The naphthenic oil is naphthenic rubber oil KN4006;The organic phosphorus compound are the nontoxic phosphite ester of powder;The alkylnaphthalene is 1- dodecyl naphthalene.The present invention can be obviously improved crude titanic chloride except vanadium speed, reach target that is energy saving and promoting product.
Description
Technical field
The invention belongs to quickly remove vanadium compounding organic matter and its system except vanadium reagents field more particularly to a kind of crude titanic chloride
Preparation Method.
Background technique
With the rapid development of economy, demand of numerous industries to titanium dioxide rapidly goes up, the domestic existing yield of high purity titanium
It is difficult to meet the market demand.In the process for refining that chloridising prepares titanium tetrachloride, need crude titanic chloride with organic except vanadium
Prolonged rectification process is carried out again after reagent mixing, and the rectifying time generally seriously affects the life of titanium white enterprise in 70~90min
Produce efficiency.Therefore, it finds a kind of quickly except vanadium reagents are the key that promote chloride process titanium dioxide production efficiency.
Patent document 1 (application number 201610585009.2) discloses a kind of method that crude titanic chloride removes vanadium, this method packet
Include: (1) crude titanic chloride by content of vanadium more than 0.3 weight % with organic except vanadium reagents first contact, and by first
It contacts obtained product to be separated by solid-liquid separation, described first contacts so that the content of vanadium being separated by solid-liquid separation in obtained liquid phase is reduced to
0.2 weight % or less;(2) step (1) is separated by solid-liquid separation to obtained liquid phase and carries out aluminium powder except vanadium.It is handled using method of the invention
The crude titanic chloride of high content of vanadium makes full use of existing aluminium powder to remove the intact device of vanadium, and level of residue is few, raw except vanadium effect is good
At solid settling property it is good.
(organic matter refines TiCl except vanadium to paper document 24Research;Author: Xu Shulin;Steel vanadium titanium (3): 28-33) it discloses
A kind of to remove vanadium reagents, in the reaction time, reaction temperature and reagent dosage are to TiCl4Influence, preferably a kind of dosage is few out, purification
The good efficient SP reagent of effect.
(crude titanic chloride organic matter removes vanadium technical study to paper document 3;Author: Yu Jing, Zhang Ping, Chen Tianxiang;Guizhou industry
College journal: natural science edition 37 (2): 29-32) disclose thick TiCl in a kind of titanium sponge production4The technique that organic matter removes vanadium
Method examines reagent dosage and reaction temperature to thick TiCl by testing the effect for comparing several organic matters and removing vanadium4Except vanadium
Influence, the result shows that self-control NR reagent is except vanadium effect is preferable, reagent dosage is few, at low cost.The smart TiCl of preparation4Vanadium content≤
0.0005%, than coloration≤5mgK2Cr2O7/L、TiCl4Content >=99.9%.
The inventors of the present invention compare the vanadium organic reagent that removes recorded in patent document 1 and paper document 1,2, respectively
Number is 1,2,3, and collects the vanadium organic reagent that removes after number and carry out the differential responses time to except vanadium influential effect is as a result, obtain
It is as follows to result:
Content of vanadium result in smart titanium under the 1 differential responses time of table
According to table 1: above-mentioned three kinds organic vanadium that remove carried out except vanadium reagents are tested, and only 2, No. 3 samples are in 90min
Reach the standard requirements of content of vanadium in smart titanium.
Therefore, people's research is distinguished according to the present invention: that records in patent document 1 and paper document 1,2 removes the organic examination of vanadium
Agent still has some problems in terms of except vanadium production efficiency.
Summary of the invention
The present invention is directed to overcome the shortage of prior art place and provide a kind of high production efficiency, it is energy saving, can the short time
Inside reach smart titanium Plays content of vanadium requirement removes vanadium organic complex oil.
The present invention also provides the preparation methods that a kind of above-mentioned crude titanic chloride quickly removes vanadium compounding organic matter.
In order to solve the above technical problems, the present invention is implemented as follows:
A kind of crude titanic chloride quickly removes vanadium compounding organic matter, including synthetic base oil, aromatic naphtha, naphthenic oil, organic
Phosphide and alkylnaphthalene.
As a preferred embodiment, synthetic base oil of the present invention, aromatic naphtha, naphthenic oil, organic phosphorus compound and alkyl
The mass ratio of naphthalene is successively are as follows: 40~70:2~10:20~30:2~10:5~10.
Further, synthetic base oil of the present invention is C18~C20Alpha-olefin oligomer, mass percentage is
40~70%.
Further, aromatic naphtha of the present invention is 2# aromatic naphtha;The 2# aromatic naphtha and C18~C20Alpha-olefin oligomerisation
The mass ratio of object is 3~9:45~55.Above-mentioned 2# aromatic naphtha is produced by Luoyang Jia Sheng oil product Co., Ltd.Above-mentioned aromatic naphtha can also
Using application number: the relevant technologies disclosed by 201210408478.9 are made.Certainly, other well known technology can also be used to be made.
Further, the naphthenic oil of the present invention is naphthenic rubber oil KN4006;The naphthenic rubber oil
KN4006 and C18~C20Alpha-olefin oligomer mass ratio be 25~30:45~55.Above-mentioned naphthenic rubber oil KN4006 by
The production of Hangzhou Fuda goods and materials petrochemical industry Co., Ltd.
Further, organic phosphorus compound of the present invention are phosphite ester;The phosphite ester and C18~C20Alpha-olefin
The mass ratio of oligomer is 3~9:45~55.
Further, alkylnaphthalene of the present invention is 1- dodecyl naphthalene;The 1- dodecyl naphthalene and C18~C20
Alpha-olefin oligomer mass ratio be 6~9:45~55.Above-mentioned 1- dodecyl naphthalene is by Shanghai Aladdin biochemical technology stock
The production of part Co., Ltd.
Further, phosphite ester of the present invention is the nontoxic phosphite ester of powder.
Above-mentioned crude titanic chloride quickly removes the preparation method of vanadium compounding organic matter, can implement as follows:
(1) by C18~C20Alpha-olefin oligomer mixed in proportion with phosphite ester, be placed in the high speed disperser of sealing
In, with revolving speed for 8000~12000r/min, 120~240min is stirred, mixed liquor A is obtained;
(2) mixed liquor obtained by step (1) is heated, temperature is controlled at 40~80 DEG C, is proportionally added into naphthenic rubber oil
KN4006, heat preservation recycle ball milling, make phosphite ester partial size in 50~200nm, obtain mixed liquid B;
(3) 90~120 DEG C are heated to mixed liquid B obtained by step (2), add aromatic naphtha in proportion, and with 100~
The speed of 120r/min stirs 30~60min;80 DEG C or more gradients are cooling, and cooling rate is 5 DEG C/30min, and 80 DEG C or less natural
It is cooled to room temperature;
(4) 1- dodecyl naphthalene is added into mixed liquid B, after adjusting carbon type ratio, constant temperature stirs 80min, static cold
But vanadium compounding organic matter is quickly removed to get purpose product crude titanic chloride to room temperature.
The present invention provides a kind of crude titanic chloride and quickly removes vanadium compounding organic matter, contains: C18~C20Alpha-olefin it is neat
Polymers, aromatic naphtha, naphthenic oil, organic phosphorus compound and alkylnaphthalene.Organic matter compounding is carried out according to above scheme.Sample is obtained thick
Reach content of vanadium standard requirements in smart titanium in titanium tetrachloride process for refining in short time, this is because in titanium tetrachloride environment,
Following reaction occurs:
Due to C18~C20Alpha-olefin oligomer refer to double bond in the oily liquids polymer of strand end, in tetrachloro
Change the hydrogen that titanium is catalyzed on the carbon of its lower end α position to be seized, carbonium ion is generated, such as formula (1).The carbonium ion of generation can be with cycloalkane
Hydrogen migration occurs, ultimately produces the aromatic hydrocarbons structure of stable structure, such as formula (2), while carbonium ion can promote aromatic hydrocarbons and be condensed
Raw carbon, such as formula (3), the raw carbon of alkylnaphthalene reacts same aromatic hydrocarbons, and organic phosphorus compound can reduce Carbon deposition, promote carbon particle dispersion, again
The oxygen in air can be captured, carbon is promoted to generate, while preventing reaction process from generating organic radicals, increases contact of the carbon with impurity
Area improves the reaction speed of carbon and impurity, organic except vanadium reagents compared to other, provided by the invention to remove vanadium organic complex
The oil time required when reaching in crude titanic chloride purification except vanadium standard is reduced to 50min by 90min (factory's rectifying time),
Therefore, above scheme can fast fast-growing carbon, have the function that quickly to remove vanadium.
The present invention can promote the removal speed of vanadium in titanium tetrachloride except vanadium compounding organic matter, make the titanium tetrachloride vanadium removal time
In 50min, content of vanadium reaches 1ppm hereinafter, saving the production energy, and the titanium tetrachloride after purification can satisfy product quality and want
It asks.
Specific embodiment
Crude titanic chloride of the present invention quickly removes vanadium compounding organic matter and contains: synthetic base oil, naphthenic oil, has aromatic naphtha
Machine phosphide and alkylnaphthalene.
Wherein, above-mentioned crude titanic chloride quickly removes in vanadium compounding organic matter, and the synthetic base oil is C18~C20's
Alpha-olefin oligomer, quality accounting is 40~70% in compounding organic matter.
Wherein, above-mentioned crude titanic chloride quickly removes in vanadium compounding organic matter, and the aromatic naphtha is 2# aromatic naphtha, multiple
With in organic matter with C18~C20Alpha-olefin oligomer mass ratio be 3~9:45~55.
Wherein, above-mentioned crude titanic chloride quickly removes in vanadium compounding organic matter, and the naphthenic oil is naphthenic rubber oil
KN4006, compounding organic matter in C18~C20Alpha-olefin oligomer mass ratio be 25~30:45~55.
Wherein, above-mentioned crude titanic chloride quickly removes in vanadium compounding organic matter, and the organic phosphorus compound are phosphite ester,
Compounding organic matter in C18~C20Alpha-olefin oligomer mass ratio be 3~9:45~55.
Wherein, above-mentioned crude titanic chloride quickly removes in vanadium compounding organic matter, and the alkylnaphthalene is 1- dodecyl naphthalene,
Its compounding organic matter in C18~C20Alpha-olefin oligomer mass ratio be 6~9:45~55.
Explanation will be further explained to a specific embodiment of the invention by embodiment below, but not indicate to send out this
Bright protection scope is limited in range described in embodiment.
Embodiment
The physical index of the compounding each ingredient of organic matter of table 2
Table 2 is the main physical index for compounding each ingredient of organic matter, compound organic matter the preparation method is as follows:
(1) by C18~C20Alpha-olefin oligomer mixed in proportion with phosphite ester, be placed in the high speed disperser of sealing
In, 10000r/min stirs 180min, obtains mixed liquor A;
(2) step (1) mixed liquor A being heated, temperature is controlled at 50 DEG C, it is proportionally added into naphthenic rubber oil KN4006,
Soak cycles ball milling makes powder phosphite ester partial size in 120nm, obtains mixed liquid B;
(3) 100 DEG C are heated to mixed liquid B obtained by step (2), add aromatic naphtha, and in proportion with the speed of 120r/min
Degree stirring 50min;80 DEG C or more gradients are cooling, and cooling rate is 5 DEG C/30min, 80 DEG C or less cooled to room temperatures;
(4) 1- dodecyl naphthalene is added into mixed liquid B, after being adjusted to required carbon type ratio, constant temperature stirring
80min is static to be cooled to room temperature to get purpose product.
Except raw material object and its content are there are in addition to multiple choices in embodiment 1, embodiment 2 and embodiment 3, other reaction conditions
And parameter is completely the same.
Table 3 is compounding organic components, physical index and effect assessment, it is in table 3 evaluation method is as follows:
The thick carbon tetrachloride 200ml of measurement vanadium content 238ppm, addition embodiment compounding oil 1ml, and cold conditions stirring 90~
Then 120min is distilled at 130~140 DEG C, collect smart titanium sample, and carry out content of vanadium and colorimetric detection.Detection knot
Content of vanadium is less than 1ppm in fruit, and coloration is lower than 5mgK2Cr2O7/L-1When be qualified product.
In conclusion the ratio of base oil, aromatic naphtha and naphthenic oil is 45~55:6~14:25 in compound proportion
~30, best proportion should be 48~50:8~12:25~30.According to carbon type analysis result it is found that the content of different carbon type is to removing
Vanadium influential effect is obvious.%CP content is 53.7~59.8 in compounding organic matter, %CN content is 26.9~33.7, %CA contains
Vanadium removal amount is big when amount is 8.8~14.7, coloration is low, at this time except vanadium effect is optimal.When %CP too high levels, carbonium ion accounting
Height, %CN, %CA content are too low, and cycloalkane and aromatic hydrocarbon accounting are low, be condensed raw carbon reaction carry out it is very fast, but final carbon amounts compared with
It is few, cause carbon to the poor removal effect of impurity.When %CN, %CA too high levels, cycloalkane and aromatic hydrocarbon accounting are high, %CP accounting
Less, the carbonium ion of generation is less, it is suppressed that cycloalkane, aromatic hydrocarbons are condensed raw carbon reaction, cause raw carbon speed to slow down, cause to remove
Vanadium speed is slow.And the sample viscosity that aromatic hydrocarbons additive amount excessively obtains is big, influences experiment process.
Table 3 compounds organic components, physical index and effect assessment
Refining titanic chloride experiment is carried out than the organic matter of preparation by above-mentioned optimal compounding, is in distillation time respectively
Smart titanium sample is collected when 50min, 60min, 70min, 90min, and carries out content of vanadium detection.
The smart titanium sample collected in embodiment is analyzed, it is as shown in table 4 to obtain experimental result.
Table 4 compounds organic matter except content of vanadium result in titanium smart after vanadium
It, can be quick by embodiment it is found that a kind of crude titanic chloride provided by the invention quickly removes in vanadium compounding organic matter
Remove VOCl in titanium tetrachloride3Impurity, in the case where reaching titanium tetrachloride purified product requirement, factory's titanium tetrachloride Refining times by
90min shortens to 50min, and be obviously improved crude titanic chloride removes vanadium speed, reaches target that is energy saving and promoting product.
It is understood that for those of ordinary skill in the art, can do in accordance with the technical idea of the present invention
Various other changes and modifications out, and all these changes and deformation all should belong to the protection model of the claims in the present invention
It encloses.
Claims (10)
1. a kind of crude titanic chloride quickly removes vanadium compounding organic matter, which is characterized in that including synthetic base oil, aromatic naphtha, ring
Alkane oil, organic phosphorus compound and alkylnaphthalene.
2. crude titanic chloride according to claim 1 quickly removes vanadium compounding organic matter, it is characterised in that: the synthesis base
Plinth oil, aromatic naphtha, naphthenic oil, organic phosphorus compound and alkylnaphthalene mass ratio successively are as follows: 40~70:2~10:20~30:2~
10:5~10.
3. crude titanic chloride according to claim 2 quickly removes vanadium compounding organic matter, it is characterised in that: the synthesis base
Plinth oil is alpha-olefin oligomer, and mass percentage is 40~70%.
4. crude titanic chloride according to claim 3 quickly removes vanadium compounding organic matter, it is characterised in that: the synthesis base
Plinth oil is C18~C20Alpha-olefin oligomer.
5. crude titanic chloride according to claim 4 quickly removes vanadium compounding organic matter, it is characterised in that: the aromatic naphtha
For 2# aromatic naphtha;The mass ratio of the aromatic naphtha and alpha-olefin oligomer is 3~9:45~55.
6. crude titanic chloride according to claim 5 quickly removes vanadium compounding organic matter, it is characterised in that: the naphthenic oil
For naphthenic rubber oil KN4006;Naphthenic rubber the oil KN4006 and C18~C20The mass ratio of alpha-olefin oligomer be
25~30:45~55.
7. crude titanic chloride according to claim 6 quickly removes vanadium compounding organic matter, it is characterised in that: described organic phosphorus
Compound is phosphite ester;The phosphite ester and C18~C20Alpha-olefin oligomer mass ratio be 3~9:45~55.
8. crude titanic chloride according to claim 7 quickly removes vanadium compounding organic matter, it is characterised in that: the alkylnaphthalene
For 1- dodecyl naphthalene;The 1- dodecyl naphthalene and C18~C20Alpha-olefin oligomer mass ratio be 6~9:45~
55。
9. any crude titanic chloride quickly removes vanadium compounding organic matter according to claim 1~8, it is characterised in that: institute
Stating phosphite ester is the nontoxic phosphite ester of powder.
10. crude titanic chloride according to claim 9 quickly removes the preparation method of vanadium compounding organic matter, feature exists
In implementation as follows:
(1) by C18~C20Alpha-olefin oligomer mixed in proportion with phosphite ester, be placed in the high speed disperser of sealing, with turn
Speed is 8000~12000r/min, stirs 120~240min, obtains mixed liquor A;
(2) mixed liquor A obtained by step (1) is heated, temperature is controlled at 40~80 DEG C, is proportionally added into naphthenic rubber oil
KN4006, heat preservation recycle ball milling, make phosphite ester partial size in 50~200nm, obtain mixed liquid B;
(3) mixed liquid B obtained by step (2) is heated to 90~120 DEG C, adds aromatic naphtha, and in proportion with 100~120r/min
Speed stir 30~60min;80 DEG C or more gradients are cooling, and cooling rate is 5 DEG C/30min, and 80 DEG C or less naturally cool to room
Temperature;
(4) 1- dodecyl naphthalene is added into mixed liquid B, after adjusting carbon type ratio, constant temperature stirs 80min, static to be cooled to
Room temperature quickly removes vanadium compounding organic matter to get purpose product crude titanic chloride.
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