CN110054217B - Compound organic matter for quickly removing vanadium from crude titanium tetrachloride and preparation method thereof - Google Patents

Compound organic matter for quickly removing vanadium from crude titanium tetrachloride and preparation method thereof Download PDF

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CN110054217B
CN110054217B CN201910352268.4A CN201910352268A CN110054217B CN 110054217 B CN110054217 B CN 110054217B CN 201910352268 A CN201910352268 A CN 201910352268A CN 110054217 B CN110054217 B CN 110054217B
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titanium tetrachloride
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vanadium
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鄂涛
肖鑫宇
杨姝宜
邢振强
刘琳
钱建华
马增英
程颖
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Bohai University
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    • C01G23/00—Compounds of titanium
    • C01G23/02—Halides of titanium
    • C01G23/022—Titanium tetrachloride
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Abstract

The invention belongs to the field of vanadium removal reagents, and particularly relates to a compound organic matter for quickly removing vanadium from crude titanium tetrachloride and a preparation method thereof, wherein the compound organic matter comprises synthetic base oil, aromatic oil, naphthenic oil, organic phosphide and alkyl naphthalene; the synthetic base oil, the aromatic oil, the naphthenic oil, the organic phosphide and the alkyl naphthalene are sequentially in mass ratio as follows: 40-70: 2-10: 20-30: 2-10: 5-10. The synthetic base oil is C18～C20An alpha-olefin oligomer of (a); the aromatic oil is 2# aromatic oil; the naphthenic oil is naphthenic base rubber oil KN 4006; the organic phosphide is powder nontoxic phosphite ester; the alkyl naphthalene is 1-n-dodecyl naphthalene. The method can obviously improve the vanadium removal speed of the crude titanium tetrachloride, and achieve the aims of saving energy and improving products.

Description

Compound organic matter for quickly removing vanadium from crude titanium tetrachloride and preparation method thereof
Technical Field
The invention belongs to the field of vanadium removal reagents, and particularly relates to a compound organic matter for quickly removing vanadium from crude titanium tetrachloride and a preparation method thereof.
Background
With the rapid development of economy, the demand of various industries on titanium dioxide is rapidly increased, and the current yield of domestic high-purity titanium cannot meet the market demand. In the refining process for preparing titanium tetrachloride by a chlorination method, a long-time rectification process is required after crude titanium tetrachloride and an organic vanadium removal reagent are mixed, the rectification time is generally 70-90 min, and the production efficiency of a titanium white enterprise is seriously influenced. Therefore, the key point for improving the production efficiency of titanium white by a chlorination process is to find a reagent for quickly removing vanadium.
Patent document 1 (application No. 201610585009.2) discloses a method for removing vanadium from crude titanium tetrachloride, which comprises: (1) carrying out first contact on crude titanium tetrachloride with the vanadium content of more than 0.3 wt% and an organic vanadium removal reagent, and carrying out solid-liquid separation on a product obtained by the first contact, wherein the vanadium content in a liquid phase obtained by the solid-liquid separation is reduced to be less than 0.2 wt% by the first contact; (2) and (3) carrying out aluminum powder vanadium removal on the liquid phase obtained by the solid-liquid separation in the step (1). The method for treating the crude titanium tetrachloride with high vanadium content fully utilizes the existing complete device for removing vanadium from aluminum powder, has the advantages of less residue, good vanadium removal effect and good settling property of the generated solid.
Paper document 2 (refining TiCl for organic vanadium removal)4Researching; the authors: a permissive forest; steel vanadium-titanium (3):28-33) discloses a vanadium removing reagent, reaction time, reaction temperature and reagent dosage for TiCl4The efficient SP reagent with small dosage and good refining effect is preferably selected.
Paper document 3 (research on vanadium removal process of crude titanium tetrachloride organic matter; author: quiet, chapter-Ping, Chentianxiang; written journal of Guizhou Industrial university: Nature edition 37(2):29-32) discloses crude TiCl in production of titanium sponge4The process method for removing vanadium from organic matters compares the vanadium removing effect of a plurality of organic matters through tests, and examines the dosage of reagents and the reaction temperature for coarse TiCl4The result shows that the self-made NR reagent has better vanadium removal effect, less reagent dosage and low cost. Prepared refined TiCl4The vanadium content is less than or equal to 0.0005 percent, and the colorimetric degree is less than or equal to 5mgK2Cr2O7/L、TiCl4The content is more than or equal to 99.9 percent.
The inventors of the present invention compare the vanadium removal organic reagents described in patent document 1 and paper documents 1 and 2, respectively numbered 1, 2 and 3, and collect the results of the different reaction times of the numbered vanadium removal organic reagents on the vanadium removal effect, and obtain the following results:
TABLE 1 results of vanadium content in refined titanium at different reaction times
Figure BDA0002044301300000021
From table 1, it can be seen that: in the vanadium removal experiment performed by the three organic vanadium removal reagents, only the No. 2 and No. 3 samples reach the standard requirement of the vanadium content in the refined titanium within 90 min.
Therefore, the inventors have found, according to their studies, that: the vanadium removal organic reagent described in patent document 1 and article documents 1 and 2 has a certain problem in terms of vanadium removal production efficiency.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the organic compound oil for removing vanadium, which has high production efficiency, saves energy and can meet the requirement of standard vanadium content in refined titanium in a short time.
The invention also provides a preparation method of the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride.
In order to solve the technical problem, the invention is realized as follows:
a compound organic matter for quickly removing vanadium from coarse titanium tetrachloride comprises synthetic base oil, aromatic oil, naphthenic oil, organic phosphide and alkyl naphthalene.
As a preferred scheme, the synthetic base oil, the aromatic oil, the naphthenic oil, the organic phosphide and the alkyl naphthalene have the following mass ratios in sequence: 40-70: 2-10: 20-30: 2-10: 5-10.
Further, the synthetic base oil of the invention is C18～C20The alpha-olefin oligomer is 40-70% by mass.
Further, the aromatic oil is 2# aromatic oil; the 2# aromatic oil and C18～C20The mass ratio of the alpha-olefin oligomer is 3-9: 45-55. The aromatic oil 2# is produced by Luoyangjia sanden oil products Co. The aromatic oils mentioned above may also be used in the applications No.: 201210408478.9, respectively, are disclosed. Of course, other known techniques may be used.
Further, the naphthenic oil is naphthenic base rubber oil KN 4006; the naphthenic base rubber oil KN4006 and C18～C20The mass ratio of the alpha-olefin oligomer is 25-30: 45 ℃55. The naphthenic base rubber oil KN4006 is produced by Hangzhou Fuda materials petrochemical company.
Further, the organic phosphide is phosphite ester; the phosphite ester and C18～C20The mass ratio of the alpha-olefin oligomer is 3-9: 45-55.
Further, the alkyl naphthalene is 1-n-dodecyl naphthalene; the 1-n-dodecylnaphthalene and C18～C20The mass ratio of the alpha-olefin oligomer is 6-9: 45-55. The 1-n-dodecylnaphthalene is produced by Shanghai Aladdin Biotechnology Ltd.
Further, the phosphite ester is powder nontoxic phosphite ester.
The preparation method of the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride can be implemented according to the following steps:
(1) c is to be18～C20The alpha-olefin oligomer and phosphite ester are mixed in proportion, placed in a sealed high-speed dispersion machine, and stirred for 120-240 min at the rotating speed of 8000-12000 r/min to obtain a mixed solution A;
(2) heating the mixed solution obtained in the step (1), controlling the temperature at 40-80 ℃, adding naphthenic base rubber oil KN4006 in proportion, preserving heat, and performing circulating ball milling to enable the particle size of phosphite ester to be 50-200 nm to obtain mixed solution B;
(3) heating the mixed solution B obtained in the step (2) to 90-120 ℃, adding aromatic oil in proportion, and stirring at the speed of 100-120 r/min for 30-60 min; gradient cooling at 80 deg.C or above at a cooling rate of 5 deg.C/30 min, and naturally cooling below 80 deg.C to room temperature;
(4) adding 1-n-dodecylnaphthalene into the mixed solution B, adjusting the carbon type ratio, stirring at constant temperature for 80min, standing and cooling to room temperature to obtain the target product, namely the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride.
The invention provides a compound organic matter for quickly removing vanadium from crude titanium tetrachloride, which comprises the following components in percentage by weight: c18～C20Alpha-olefin oligomers, aromatic oils, naphthenic oils, organophosphates and alkylnaphthalenes. And (4) compounding organic matters according to the scheme. The obtained sample is subjected to crude tetrachloro reactionThe standard requirement of vanadium content in refined titanium is met in a short time in the titanium refining process, because the following reactions occur in the titanium tetrachloride environment:
Figure BDA0002044301300000041
Figure BDA0002044301300000042
Figure BDA0002044301300000043
due to C18～C20The alpha-olefin oligomer refers to an oily liquid polymer with double bonds at the ends of molecular chains, and hydrogen on alpha-terminal carbon of the oily liquid polymer is abstracted under the catalysis of titanium tetrachloride to generate a carbocation, as shown in the formula (1). The generated carbenium ion can generate hydrogen transfer with cyclane, and finally generate an aromatic hydrocarbon structure with a stable structure, as shown in formula (2), and simultaneously the carbenium ion can promote the aromatic hydrocarbon to generate condensed carbon, as shown in formula (3), the alkyl naphthalene carbon generation reaction is reacted with the aromatic hydrocarbon, and the organic phosphide can reduce carbon deposition, promote carbon particle dispersion, capture oxygen in the air, promote carbon generation, prevent organic matter groups from being generated in the reaction process, increase the contact area of carbon and impurities, and improve the reaction speed of carbon and impurities.
The compound organic matter for removing vanadium can improve the removal speed of vanadium in titanium tetrachloride, so that the vanadium content of the titanium tetrachloride reaches below 1ppm when the vanadium removal time of the titanium tetrachloride is 50min, the production energy is saved, and the refined titanium tetrachloride can meet the product quality requirement.
Detailed Description
The compound organic matter for quickly removing vanadium from crude titanium tetrachloride comprises: synthetic base oil, aromatic oil, naphthenic oil, organic phosphide and alkyl naphthalene.
Wherein, in the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride, the synthetic base oil is C18～C20The mass percentage of the alpha-olefin oligomer in the compound organic matter is 40-70%.
Wherein, in the compound organic matter for rapidly removing vanadium from the crude titanium tetrachloride, the aromatic oil is 2# aromatic oil which is mixed with C in the compound organic matter18～C20The mass ratio of the alpha-olefin oligomer is 3-9: 45-55.
Wherein, in the compound organic matter for rapidly removing vanadium from the crude titanium tetrachloride, the naphthenic oil is naphthenic base rubber oil KN4006 which is mixed with C in the compound organic matter18～C20The mass ratio of the alpha-olefin oligomer is 25-30: 45-55.
Wherein, in the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride, the organic phosphide is phosphite ester which is mixed with C in the compound organic matter18～C20The mass ratio of the alpha-olefin oligomer is 3-9: 45-55.
Wherein, in the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride, the alkyl naphthalene is 1-n-dodecyl naphthalene which is mixed with C in the compound organic matter18～C20The mass ratio of the alpha-olefin oligomer is 6-9: 45-55.
The following examples further illustrate specific embodiments of the present invention, but are not intended to limit the scope of the invention to those described in the examples.
Examples
TABLE 2 physical property indexes of each component of the compound organic matter
Figure BDA0002044301300000061
Table 2 shows the main physical property indexes of the components of the compound organic matter, and the preparation method of the compound organic matter is as follows:
(1) c is to be18～C20Of alpha-olefin oligomers withMixing phosphite esters in proportion, placing the mixture in a sealed high-speed dispersion machine at 10000r/min, and stirring for 180min to obtain a mixed solution A;
(2) heating the mixed solution A in the step (1), controlling the temperature at 50 ℃, adding naphthenic base rubber oil KN4006 in proportion, and performing heat preservation and circulating ball milling to ensure that the particle size of the powder phosphite ester is 120nm to obtain mixed solution B;
(3) heating the mixed solution B obtained in the step (2) to 100 ℃, adding aromatic oil in proportion, and stirring at the speed of 120r/min for 50 min; gradient cooling at 80 deg.C or above at a cooling rate of 5 deg.C/30 min, and naturally cooling below 80 deg.C to room temperature;
(4) adding 1-n-dodecylnaphthalene into the mixed solution B, adjusting to the required carbon type ratio, stirring at constant temperature for 80min, standing, and cooling to room temperature to obtain the target product.
Except for the various choices of raw materials and their contents, the reaction conditions and parameters were completely the same in examples 1, 2 and 3.
Table 3 shows the evaluation of the composition of the compounded organic matter, physical property indexes, and effects, and the evaluation method in table 3 is as follows:
200ml of crude carbon tetrachloride with vanadium content of 238ppm is measured, 1ml of the compound oil in the embodiment is added, the mixture is stirred for 90-120 min in a cold state, then distillation is carried out at 130-140 ℃, a refined titanium sample is collected, and vanadium content and chromaticity detection are carried out. The vanadium content in the detection result is less than 1ppm, and the chroma is less than 5mgK2Cr2O7/L-1The product is qualified.
In summary, in the compounding ratio, the ratio of the base oil, the aromatic oil and the naphthenic oil is 45-55: 6-14: 25-30, and the optimal ratio is 48-50: 8-12: 25-30. According to the analysis result of the carbon types, the content of different carbon types has obvious influence on the vanadium removal effect. When the content of the% CP is 53.7-59.8, the content of the% CN is 26.9-33.7, and the content of the% CA is 8.8-14.7 in the compound organic matter, the vanadium removal amount is large, the chroma is low, and the vanadium removal effect is optimal. When the content of the% CP is too high, the content of the carbocation is high, the content of the% CN and the% CA is too low, the content of the cycloparaffin and the aromatic hydrocarbon is low, the condensation carbon generation reaction is quicker, but the final carbon content is less, so that the removal effect of the carbon on impurities is poor. When the content of% CN and% CA is too high, the ratio of naphthenic hydrocarbon to aromatic hydrocarbon is high, the ratio of% CP is less, the generated carbocation is less, the condensation carbon generation reaction of naphthenic hydrocarbon and aromatic hydrocarbon is inhibited, the carbon generation speed is reduced, and the vanadium removal speed is slow. And the viscosity of a sample obtained by excessive addition of aromatic hydrocarbon is large, so that the experimental process is influenced.
TABLE 3 evaluation of composition of organic substances, physical index and effect
Figure BDA0002044301300000081
And (3) carrying out a titanium tetrachloride refining experiment on the organic matters prepared according to the optimal compound ratio, collecting refined titanium samples when the distillation time is 50min, 60min, 70min and 90min respectively, and detecting the content of vanadium.
The fine titanium samples collected in the examples were analyzed, and the results of the experiments are shown in table 4.
TABLE 4 results of vanadium content in refined titanium after vanadium removal from compounded organic
Figure BDA0002044301300000082
Figure BDA0002044301300000091
According to the embodiment, the VOCl in the titanium tetrachloride can be quickly removed from the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride3Impurities shorten the titanium tetrachloride refining time of a factory from 90min to 50min under the condition of meeting the requirement of a titanium tetrachloride refined product, obviously improve the vanadium removal speed of crude titanium tetrachloride, and achieve the aims of saving energy and improving the product.
It is understood that various other changes and modifications may be made by those skilled in the art based on the technical idea of the present invention, and all such changes and modifications should fall within the protective scope of the claims of the present invention.

Claims (7)

1. A compound organic matter for quickly removing vanadium from crude titanium tetrachloride is characterized by comprising synthetic base oil, aromatic oil, naphthenic oil, organic phosphide and alkyl naphthalene; the synthetic base oil, the aromatic oil, the naphthenic oil, the organic phosphide and the alkyl naphthalene are sequentially in mass ratio as follows: 40-70: 2-10: 20-30: 2-10: 5-10; the synthetic base oil is C18～C20The alpha-olefin oligomer is 40-70% by mass.
2. The compound organic matter for rapidly removing vanadium from crude titanium tetrachloride according to claim 1, which is characterized in that: the aromatic oil is 2# aromatic oil; the mass ratio of the aromatic oil to the alpha-olefin oligomer is 3-9: 45-55.
3. The compound organic matter for rapidly removing vanadium from crude titanium tetrachloride according to claim 2, which is characterized in that: the naphthenic oil is naphthenic base rubber oil KN 4006; the naphthenic base rubber oil KN4006 and C18～C20The mass ratio of the alpha-olefin oligomer is 25-30: 45-55.
4. The compound organic matter for rapidly removing vanadium from crude titanium tetrachloride according to claim 3, which is characterized in that: the organic phosphide is phosphite ester; the phosphite ester and C18～C20The mass ratio of the alpha-olefin oligomer is 3-9: 45-55.
5. The compound organic matter for rapidly removing vanadium from crude titanium tetrachloride according to claim 4, which is characterized in that: the alkyl naphthalene is 1-n-dodecyl naphthalene; the 1-n-dodecylnaphthalene and C18～C20The mass ratio of the alpha-olefin oligomer is 6-9: 45-55.
6. The compound organic matter for rapidly removing vanadium from crude titanium tetrachloride according to any one of claims 4 to 5, which is characterized in that: the phosphite ester is powder nontoxic phosphite ester.
7. The preparation method of the compound organic matter for quickly removing vanadium from crude titanium tetrachloride according to claim 5, which is characterized by comprising the following steps:
(1) c is to be18～C20The alpha-olefin oligomer and phosphite ester are mixed in proportion, placed in a sealed high-speed dispersion machine, and stirred for 120-240 min at the rotating speed of 8000-12000 r/min to obtain a mixed solution A;
(2) heating the mixed solution A obtained in the step (1), controlling the temperature to be 40-80 ℃, adding naphthenic base rubber oil KN4006 in proportion, preserving heat, and performing circulating ball milling to enable the particle size of phosphite ester to be 50-200 nm to obtain mixed solution B;
(3) heating the mixed solution B obtained in the step (2) to 90-120 ℃, adding aromatic oil in proportion, and stirring at the speed of 100-120 r/min for 30-60 min; gradient cooling at 80 deg.C or above at a cooling rate of 5 deg.C/30 min, and naturally cooling below 80 deg.C to room temperature;
(4) adding 1-n-dodecylnaphthalene into the mixed solution B, adjusting the carbon type ratio, stirring at constant temperature for 80min, standing and cooling to room temperature to obtain the target product, namely the compound organic matter for quickly removing vanadium from the crude titanium tetrachloride.
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