CN104370689B - A kind of LED material purification process of high-purity grade of methyl iodide - Google Patents
A kind of LED material purification process of high-purity grade of methyl iodide Download PDFInfo
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- CN104370689B CN104370689B CN201410558875.3A CN201410558875A CN104370689B CN 104370689 B CN104370689 B CN 104370689B CN 201410558875 A CN201410558875 A CN 201410558875A CN 104370689 B CN104370689 B CN 104370689B
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Abstract
The invention discloses the purification process of a kind of LED material high-purity grade of methyl iodide.This purification process comprises: methyl iodide crude product filters through ZSM-12 molecular sieve chelate sorbent by (1); (2) rectifier unit is adopted to carry out rectifying described filtrate; (3) described rectifying liquid is carried out ultrafiltration.ZSM-12 molecular sieve chelate sorbent is adopted to filter in purification process of the present invention, ZSM-12 molecular sieve chelate sorbent has very strong adsorptive power to the hydroxyl impurity in methyl iodide contained by crude product, free-iodine, moisture, metal ion, effectively can remove impurity wherein, thus improve the purity of product.By the methyl iodide after the filtration of ZSM-12 molecular sieve chelate sorbent successively through rectifying and ultrafiltration, can obtain LED material high-purity grade of methyl iodide, simplify operation sequence, operating process is environmental protection more, ensure that the quality of product and lower production cost simultaneously.
Description
Technical field
The present invention relates to the technical field that methyl iodide is purified, particularly relate to the purification process of a kind of LED material high-purity grade of methyl iodide.
Background technology
Methyl iodide is a halohydrocarbon, and molecular formula is written as CH
3i, be an iodine substituent of methane, it is at room temperature the volatile liquid that density is large, moment of dipole 1.59D, specific refractory power 1.5304 (20 DEG C, D), 1.5293 (21 DEG C, D).Methyl iodide can with to common are machine solvent miscible, and sterling is colourless, can decomposite elemental iodine and be with purple under being exposed to sunlight, removes by adding metallic copper.Methyl iodide is present in rice field on a small quantity.Methyl iodide is methylating reagent conventional in organic synthesis.
The common method of purification of high-purity iodine methane stirs with rare hypo solution or sodium bisulfate, then water, dilute sodium carbonate solution and more water washing is used respectively, finally namely obtain the finished product with the dry also distillation of calcium chloride, shortcoming is complex operation, washing process has greater environmental impacts, therefore inapplicable industrial applications.
Summary of the invention
In view of this, the invention provides the purification process of a kind of LED material high-purity grade of methyl iodide, this purification process has environmental protection, simple to operate, and the purity of the refined product obtained through this purification process is higher.
A LED material purification process for high-purity grade of methyl iodide, comprises the following steps:
(1) methyl iodide crude product is filtered through ZSM-12 molecular sieve chelate sorbent, obtain filtrate;
(2) adopt rectifier unit to carry out rectifying described filtrate, obtain rectifying liquid;
(3) described rectifying liquid is carried out ultrafiltration, obtain LED material high-purity grade of methyl iodide.
Here the term " adsorbent of molecular sieve " that term " molecular sieve chelate sorbent " is general with this area is same connotation.Term " methyl iodide crude product " the i.e. methyl iodide of technical grade purity, such as purity is 90 ~ 95wt%.Molecular sieve chelate sorbent of the present invention is preferably and adopts through pickling process modification, to improve the effect that it filters, certainly also to adopt without pickling process modification or additive method modification.The detailed process of this modification is, ZSM-12 molecular sieve is flooded in steeping fluid 12 ~ 24h then dry gained.Steeping fluid can for by be dissolved in by 2,4 dihydroxyl benzophenone be mixed with hexone, ethanol mixed solvent obtained by, or be dissolved in by 2,4 dihydroxyl benzophenone be mixed with hexone, ether mixed solvent obtained by.In the component of this steeping fluid, 2,4-dihydroxy benaophenonel and hexone amount ratio are 1g:(4.5 ~ 5.5) ml, 2, the amount ratio of 4-dihydroxy benaophenonel and ethanol (or ether) is 1g:(3 ~ 5) ml, certain this area other steeping fluids of being familiar be applicable to this programme too.
In rectifying, its pressure filtered is preferably 0.15 ~ 0.2MPa, and temperature is 20 ~ 25 DEG C.Rectifying is specially, first filtrate is inserted in rectifier unit 42 ~ 43 DEG C according to reflux ratio be 10:3 ~ 5 reflux 1 ~ 2h, remove front-end volatiles obtain treating rectifying liquid; Then, will treat that rectifying liquid carries out rectifying with the flow velocity of 20 ~ 30mL/min.The device of rectifying can adopt the general any one in this area to can be used for the device of distillation operation, such as quartz glass fractionating tower etc.
In ultrafiltration, ultrafiltration adopts hollow fiber ultrafiltration membrane.Hollow fiber ultrafiltration membrane is the filter membrane with hollow structure containing micropore, and the aperture of its micropore is not more than 0.05 μm.
ZSM-12 molecular sieve chelate sorbent is adopted to filter in purification process of the present invention, ZSM-12 molecular sieve chelate sorbent has very strong adsorptive power to the hydroxyl impurity in methyl iodide contained by crude product, free-iodine, moisture, metal ion, effectively can remove impurity wherein, thus improve the purity of product.By the methyl iodide after the filtration of ZSM-12 molecular sieve chelate sorbent successively through rectifying and ultrafiltration, can obtain LED material high-purity grade of methyl iodide, simplify operation sequence, operating process is environmental protection more, ensure that the quality of product and lower production cost simultaneously.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
The preparation of ZSM-12 molecular sieve chelate sorbent post: get 500g2,4-dihydroxy benaophenonel, add in 2250ml hexone, 1180ml ethanol and dissolve composition steeping fluid, at room temperature 300gZSM-12 molecular sieve is added in this steeping fluid, filter after dipping 12h, after cleaning secondary with the ultrapure water 1080ml of 18.2M Ω .cm, dry 12h at 102 DEG C, namely ZSM-12 molecular sieve chelate sorbent 400g is obtained, dress post, stand-by.
The purifying of methyl iodide crude product: be that 95.0wt% technical grade methyl iodide raw material filters through ZSM-12 molecular sieve chelate sorbent at 0.15MPa, 20 DEG C of temperature by 1000g content, filtrate is through quartz purification rectifier unit 42.5 DEG C backflow 1 ~ 2h, adjustment reflux ratio is 10:3, remove front-end volatiles, carry out rectifying with the flow velocity of 20mL/min, collect rectifying fluid and be LED material high-purity grade of methyl iodide through 0.05 μm of hollow fiber filter membrane filtration.The methyl iodide content 99.51wt% of purified product in this example, yield 91.32%, the index such as petroleum ether dissolution test, acidity, moisture in product all meets the standard of LED material high-purity grade of methyl iodide.
Embodiment 2
The preparation of ZSM-12 molecular sieve chelate sorbent post: get 500g2,4-dihydroxy benaophenonel, add in 2500ml hexone, 2360ml ethanol and dissolve composition steeping fluid, at room temperature 300gZSM-12 molecular sieve is added in this steeping fluid, filter after dipping 24h, after cleaning secondary with the ultrapure water 1080ml of 18.2M Ω .cm, dry 12h at 102 DEG C, namely ZSM-12 molecular sieve chelate sorbent 386g is obtained, dress post, stand-by.
The purifying of methyl iodide crude product: be that 95.0wt% technical grade methyl iodide raw material filters through ZSM-12 molecular sieve chelate sorbent at 0.2MPa, 25 DEG C of temperature by 1000g content, filtrate is through quartz purification rectifier unit 42.5 DEG C backflow 2h, adjustment reflux ratio is 10:5, remove front-end volatiles, carry out rectifying with the flow velocity of 30mL/min, collect rectifying fluid and be LED material high-purity grade of methyl iodide through 0.05 μm of hollow fiber filter membrane filtration.The methyl iodide content 99.67wt% of purified product in this example, yield 90.12%.After testing, the index such as petroleum ether dissolution test, acidity, moisture in product all meets the standard of LED material high-purity grade of methyl iodide.
Embodiment 3
The preparation of ZSM-12 molecular sieve chelate sorbent post: get 500g2,4-dihydroxy benaophenonel, add in 2750ml hexone, 2360ml ether and dissolve composition steeping fluid, at room temperature 300gZSM-12 molecular sieve is added in this steeping fluid, filter after dipping 24h, after cleaning secondary with the ultrapure water 1080ml of 18.2M Ω .cm, dry 12h at 102 DEG C, namely ZSM-12 molecular sieve chelate sorbent 380g is obtained, dress post, stand-by.
The purifying of methyl iodide crude product: be that 95.0wt% technical grade methyl iodide raw material filters through ZSM-12 molecular sieve chelate sorbent at 0.2MPa, 25 DEG C of temperature by 1000g content, filtrate is through quartz purification rectifier unit 42.5 DEG C backflow 2h, adjustment reflux ratio is 10:5, remove front-end volatiles, carry out rectifying with the flow velocity of 30mL/min, collect rectifying fluid and be LED material high-purity grade of methyl iodide through 0.05 μm of hollow fiber filter membrane filtration.The methyl iodide content 99.61wt% of purified product in this example, yield 90.17%.After testing, the index such as petroleum ether dissolution test, acidity, moisture in product all meets the standard of LED material high-purity grade of methyl iodide.
By the specific performance of the purified product of embodiment 1 ~ 3 as following table:
Because the numerical range of each processing parameter involved in the present invention can not all embody in the above-described embodiments, as long as but those skilled in the art can imagine any numerical value fallen in this numerical range above-mentioned completely all can implement the present invention, certainly also comprise the arbitrary combination of occurrence in some numerical ranges.Herein, for the consideration of length, eliminate the embodiment providing occurrence in certain one or more numerical range, this should not be considered as the insufficient disclosure of technical scheme of the present invention.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (9)
1. a LED material purification process for high-purity grade of methyl iodide, is characterized in that, comprise the following steps:
(1) methyl iodide crude product is filtered through ZSM-12 molecular sieve chelate sorbent, obtain filtrate;
(2) adopt rectifier unit to carry out rectifying described filtrate, obtain rectifying liquid;
(3) described rectifying liquid is carried out ultrafiltration, obtain LED material high-purity grade of methyl iodide.
2. purification process according to claim 1, is characterized in that, molecular sieve chelate sorbent described in step (1) is by ZSM-12 molecular sieve being flooded in steeping fluid 12 ~ 24h then dry gained.
3. purification process according to claim 2, it is characterized in that, described steeping fluid is by 2,4-dihydroxy benaophenonel be dissolved in be mixed with hexone, ethanol mixed solvent obtained by, or be dissolved in obtained by the mixed solvent being mixed with hexone, ether by 2,4 dihydroxyl benzophenone.
4. purification process according to claim 3, is characterized in that, described 2,4 dihydroxyl benzophenone and hexone amount ratio are 1g:(4.5 ~ 5.5) ml.
5. purification process according to claim 3, is characterized in that, described 2,4 dihydroxyl benzophenone and ethanol amount ratio are 1g:(3 ~ 5) ml, described 2,4 dihydroxyl benzophenone and ether amount ratio are 1g:(3 ~ 5) ml.
6. purification process according to claim 1, is characterized in that, the pressure filtered described in step (1) is 0.15 ~ 0.2MPa, and temperature is 20 ~ 25 DEG C.
7. purification process according to claim 1, is characterized in that, described in step (1), the purity of methyl iodide crude product is 90 ~ 95wt%.
8. purification process according to claim 1, it is characterized in that, described in step (2), rectifying is specially, first filtrate is inserted in rectifier unit 42 ~ 43 DEG C according to reflux ratio be 10:3 ~ 5 reflux 1 ~ 2h, remove front-end volatiles obtain treating rectifying liquid; Then, will treat that rectifying liquid carries out rectifying with the flow velocity of 20 ~ 30mL/min.
9. purification process according to claim 1, is characterized in that, ultrafiltration described in step (3) adopts aperture to be not more than the hollow fiber ultrafiltration membrane of 0.05 μm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6008421A (en) * | 1994-11-14 | 1999-12-28 | Larsen; Peter | Production of 11 C-methyl iodide |
| CN1769252A (en) * | 2003-07-02 | 2006-05-10 | 日宝化学株式会社 | Alkyl iodide recovery method and alkyl iodide recovery apparatus |
| CN102295519A (en) * | 2011-07-26 | 2011-12-28 | 太仓沪试试剂有限公司 | Preparation method for iodomethane |
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- 2014-10-20 CN CN201410558875.3A patent/CN104370689B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6008421A (en) * | 1994-11-14 | 1999-12-28 | Larsen; Peter | Production of 11 C-methyl iodide |
| CN1769252A (en) * | 2003-07-02 | 2006-05-10 | 日宝化学株式会社 | Alkyl iodide recovery method and alkyl iodide recovery apparatus |
| CN102295519A (en) * | 2011-07-26 | 2011-12-28 | 太仓沪试试剂有限公司 | Preparation method for iodomethane |
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