CN105254654A - Method for purifying alkyl indium - Google Patents
Method for purifying alkyl indium Download PDFInfo
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- CN105254654A CN105254654A CN201510798429.4A CN201510798429A CN105254654A CN 105254654 A CN105254654 A CN 105254654A CN 201510798429 A CN201510798429 A CN 201510798429A CN 105254654 A CN105254654 A CN 105254654A
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Abstract
The invention belongs to a method for purifying alkyl indium, which comprises the following steps: (1) complex replacement reaction: under the protection of inert gas, adding phosphine ligands into a reaction kettle, then adding alkyl indium and ether complexes under the condition of stirring, and continuing to stir for 1-5 hours to carry out replacement reaction; (2) ether recovery: under the conditions that the vacuum degree is 100-600 mmHg and the temperature is 60-120 DEG C, distilling for 5-15 h so as to recover ethers replaced out in the replacement reaction; (3) impurity removal: under the conditions that the vacuum degree is 1-100 mmHg and the temperature is 60-120 DEG C, distilling for 4-20 h so as to remove ethers and low-boiling-point impurities; (4) deolation: under the conditions that the vacuum degree is 1-100 mmHg and the temperature is 100-220 DEG C, carrying out deolation so as to obtain an alkyl indium crude product; and (5) rectification: feeding the alkyl indium crude product into a rectifying tower to rectify, so that high-purity alkyl indium is obtained. The method disclosed by the invention avoids the defects existing when high-polyether ligands and amine ligands are used, and the method is good in impurity removal effect, and reduces the requirements of the rectification process on distillation equipment and processes.
Description
Technical field
The invention belongs to alkyl indium purification techniques field, be specifically related to a kind of method of purification of alkyl indium.
Background technology
High-purity metal organic compound (being called for short MO source) is one of most critical basic material growing photoelectricity semiconductor film material in metal organic chemical vapor deposition technology (MOCVD), chemical beam epitaxy technology (CBE) process.Wherein, high-purity metal organic compound alkyl indium (trimethyl indium, triethylindium and ethyl dimethyl indium) is the organo indium source of the thin-film materials such as growing gallium nitride indium (InGaN), Gallium indium arsenide (InGaAs), InGaP (InGaP) and indium phosphide (InP), is also one of raw material that most important, consumption is maximum at present.Metal organic chemical vapor deposition technology (MOCVD) is high especially to the purity requirement in MO source, requires that its purity is more than or equal to 99.9999%(6N).Especially, along with MOCVD technology constantly develops, require that the impurity content that some responsive difficulty of MO source is removed is lower, as impurity such as Zn, Si, Fe, O, this purifying technique to MO source proposes higher requirement.
The Xie Peiyu of current alkyl indium and etherate conventional method of purifying mainly uses high polyethers part and amine part solution to join, then rectification and purification.The equal Shortcomings of above two class part, high polyethers part is: 1) easily sex change occurs in solution timing; 2) alkyl indium oxygen level is higher; 3) product loss is large.Amine part is: 1) part is easily distilled out of with product, and product purity is low, and rectifying pressure is large; 2) need to carry out repeatedly solution to join, production efficiency is low.
Summary of the invention
The object of this invention is to provide that a kind of technique is simple, refining effect good, be applicable to the method for purification of the alkyl indium of large-scale production.
For achieving the above object, the technical solution used in the present invention is, a kind of method of purification of alkyl indium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under protection of inert gas, adds phosphine class part in reactor, then adds alkyl indium and ethers title complex under agitation, continues stirring and carries out replacement(metathesis)reaction in 1 ~ 5 hour;
2. ethers reclaims: at vacuum tightness 100 ~ 600mmHg, temperature 60 ~ 120 DEG C, distill the ethers that 5 ~ 15h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 4 ~ 20h and remove ether and lower-boiling impurity at vacuum tightness 1 ~ 100mmHg, temperature 60 ~ 120 DEG C;
4. solution is joined: at vacuum tightness 1 ~ 100mmHg, temperature 100 ~ 220 DEG C, solution joins acquisition alkyl indium crude product;
5. rectifying: alkyl indium crude product is sent into rectifying tower rectifying and obtains high-purity alkyl indium.
The mol ratio of described alkyl indium and ethers title complex, phosphine class part is 1:1 ~ 3.
Described phosphine class part is triphenylphosphine or alkylphosphines; Wherein, the alkyl in alkylphosphines is the alkyl of C atomicity 4-8.
Ethers in described alkyl indium and ethers title complex is ether or tetrahydrofuran (THF).
Step 5. described in the pressure of rectifying tower be 200 ~ 500mmHg, column bottom temperature 100 ~ 160 DEG C, reflux ratio 5 ~ 20:1.
Described step 5. in rectifying tower used be packing tower.
Described step 5. in rectifying tower used be packing tower.
The filler of described packing tower adopts the loose filler of heap or structured packing; The loose filler of heap is any shape, such as but not limited to ring-type, saddle, waved plate etc., is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 10 ~ 60.
The beneficial effect that the present invention produces is: present invention, avoiding the shortcoming existed when using high polyethers part and amine part, and good impurity removing effect, greatly reduce the requirement of rectification working process to rectifying device and rectification process, effectively improve production efficiency, be more suitable for large-scale production; Adopt the solution of phosphine class part to alkyl indium and ethers title complex to match the impurity element removed in responsive difficulty, as better effects if such as Zn, Si, Fe, O, improve quality and the stability of product; Solution joins the ether solvent and the equal reusable edible of phosphine class part used that reclaim in process, saves the discharge of production cost and minimizing " three wastes " significantly.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited thereto.
Embodiment 1
A method of purification for trimethyl indium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, triphenylphosphine is added in reactor, then add trimethyl indium and etherate (mol ratio of trimethyl indium and etherate, triphenylphosphine is 1:1) under agitation, continue stirring and carry out replacement(metathesis)reaction in 2 hours;
2. ethers reclaims: at vacuum tightness 300mmHg, temperature 90 DEG C, distill the ether that 10h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 10h and remove ether and lower-boiling impurity at vacuum tightness 50mmHg, temperature 90 DEG C;
4. solution is joined: at vacuum tightness 60mmHg, temperature 160 DEG C, solution joins acquisition trimethyl indium crude product;
5. rectifying: trimethyl indium crude product is sent into rectifying tower rectifying and obtains high-purity trimethyl indium (purity >=99.9999%), the pressure of rectifying tower is 300mmHg, column bottom temperature 30 DEG C, reflux ratio 12:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is ring-type, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 30.
In the present embodiment, the yield of trimethyl indium is 90%.
Embodiment 2
A method of purification for triethylindium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, triphenylphosphine is added in reactor, then add triethylindium and etherate (mol ratio of triethylindium and etherate, triphenylphosphine is 1:3) under agitation, continue stirring and carry out replacement(metathesis)reaction in 1 hour;
2. ethers reclaims: at vacuum tightness 100mmHg, temperature 120 DEG C, distill the ether that 5h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 4h and remove ether and lower-boiling impurity under vacuum tightness 50mmHg, temperature 60 C;
4. solution is joined: at vacuum tightness 100mmHg, temperature 100 DEG C, solution joins acquisition triethylindium crude product;
5. rectifying: triethylindium crude product is sent into rectifying tower rectifying and obtains high-purity triethylindium (purity >=99.9999%), the pressure of rectifying tower is 200mmHg, column bottom temperature 160 DEG C, reflux ratio 5:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is saddle, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 10.
In the present embodiment, the yield of triethylindium is 86.9%.
Embodiment 3
A method of purification for triethylindium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, triphenylphosphine is added in reactor, then add triethylindium and etherate (mol ratio of triethylindium and etherate, triphenylphosphine is 1:2) under agitation, continue stirring and carry out replacement(metathesis)reaction in 3 hours;
2. ethers reclaims: under vacuum tightness 600mmHg, temperature 60 C, distill the ether that 15h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 20h and remove ether and lower-boiling impurity at vacuum tightness 1mmHg, temperature 120 DEG C;
4. solution is joined: at vacuum tightness 1mmHg, temperature 220 DEG C, solution joins acquisition triethylindium crude product;
5. rectifying: triethylindium crude product is sent into rectifying tower rectifying and obtains high-purity triethylindium (purity >=99.9999%), the pressure of rectifying tower is 500mmHg, column bottom temperature 100 DEG C, reflux ratio 20:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is waved plate, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 60.
In the present embodiment, the yield of triethylindium is 88.9%.
Embodiment 4
A method of purification for trimethyl indium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, three n-hexyl phosphines are added in reactor, then add trimethyl indium and etherate (mol ratio of trimethyl indium and etherate, three n-hexyl phosphines is 1:1.5) under agitation, continue stirring and carry out replacement(metathesis)reaction in 3 hours;
2. ethers reclaims: at vacuum tightness 200mmHg, temperature 80 DEG C, distill the ether that 8h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 10h and remove ether and lower-boiling impurity under vacuum tightness 20mmHg, temperature 70 C;
4. solution is joined: at vacuum tightness 20mmHg, temperature 120 DEG C, solution joins acquisition trimethyl indium crude product;
5. rectifying: trimethyl indium crude product is sent into rectifying tower rectifying and obtains high-purity trimethyl indium (purity >=99.9999%), the pressure of rectifying tower is 400mmHg, column bottom temperature 110 DEG C, reflux ratio 15:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap or structured packing; The loose filler of heap is ring-type, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 30.
In the present embodiment, the yield of trimethyl indium is 91.2%.
Embodiment 5
A method of purification for triethylindium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, three n-hexyl phosphines are added in reactor, then add triethylindium and etherate (mol ratio of triethylindium and etherate, three n-hexyl phosphines is 1:2.5) under agitation, continue stirring and carry out replacement(metathesis)reaction in 4 hours;
2. ethers reclaims: at vacuum tightness 400mmHg, temperature 110 DEG C, distill the ether that 6h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 12h and remove ether and lower-boiling impurity at vacuum tightness 30mmHg, temperature 100 DEG C;
4. solution is joined: at vacuum tightness 30mmHg, temperature 160 DEG C, solution joins acquisition triethylindium crude product;
5. rectifying: triethylindium crude product is sent into rectifying tower rectifying and obtains high-purity triethylindium (purity >=99.9999%), the pressure of rectifying tower is 2500mmHg, column bottom temperature 150 DEG C, reflux ratio 8:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is ring-type, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 20.
In the present embodiment, the yield of triethylindium is 87.2%.
Embodiment 6
A method of purification for ethyl dimethyl indium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, three n-hexyl phosphines are added in reactor, then add ethyl dimethyl indium and tetrahydrofuran (THF) title complex (mol ratio of ethyl dimethyl indium and tetrahydrofuran (THF) title complex, three n-hexyl phosphines is 1:1 ~ 3) under agitation, continue stirring and carry out replacement(metathesis)reaction in 5 hours;
2. ethers reclaims: at vacuum tightness 100mmHg, temperature 75 DEG C, distill the tetrahydrofuran (THF) that 13h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 16h and remove tetrahydrofuran (THF) and lower-boiling impurity at vacuum tightness 20mmHg, temperature 90 DEG C;
4. solution is joined: at vacuum tightness 50mmHg, temperature 200 DEG C, solution joins acquisition ethyl dimethyl indium crude product;
5. rectifying: ethyl dimethyl indium crude product is sent into rectifying tower rectifying and obtains high-purity ethyl dimethyl indium (purity >=99.9999%, yield is 89.2%), the pressure of rectifying tower is 350mmHg, column bottom temperature 135 DEG C, reflux ratio 9:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is saddle, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 40.
In the present embodiment, the yield of ethyl dimethyl indium is 89.2%.
Embodiment 7
A method of purification for trimethyl indium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, tri-n-octyl phosphine is added in reactor, then add trimethyl indium and etherate (mol ratio of trimethyl indium and etherate, tri-n-octyl phosphine is 1:2.5) under agitation, continue stirring and carry out replacement(metathesis)reaction in 2 hours;
2. ethers reclaims: at vacuum tightness 500mmHg, temperature 75 DEG C, distill the ether that 9h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 4 ~ 20 removing ether and lower-boiling impurities at vacuum tightness 30mmHg, temperature 75 DEG C;
4. solution is joined: at vacuum tightness 50mmHg, temperature 160 DEG C, solution joins acquisition trimethyl indium crude product;
5. rectifying: trimethyl indium crude product is sent into rectifying tower rectifying and obtains high-purity trimethyl indium (purity >=99.9999%), the pressure of rectifying tower is 450mmHg, column bottom temperature 125 DEG C, reflux ratio 18:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is waved plate, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 50.
In the present embodiment, the yield of trimethyl indium is 90.8%.
Embodiment 8
A method of purification for triethylindium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, tri-n-octyl phosphine is added in reactor, then add triethylindium and etherate (mol ratio of triethylindium and etherate, tri-n-octyl phosphine is 1:1) under agitation, continue stirring and carry out replacement(metathesis)reaction in 2 hours;
2. ethers reclaims: at vacuum tightness 250mmHg, temperature 80 DEG C, distill the ether that 6h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 4 ~ 20 removing ether and lower-boiling impurities at vacuum tightness 30mmHg, temperature 90 DEG C;
4. solution is joined: at vacuum tightness 70mmHg, temperature 180 DEG C, solution joins acquisition triethylindium crude product;
5. rectifying: triethylindium crude product is sent into rectifying tower rectifying and obtains high-purity triethylindium (purity >=99.9999%), the pressure of rectifying tower is 380mmHg, column bottom temperature 115 DEG C, reflux ratio 19:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is ring-type, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 45.
In the present embodiment, the yield of triethylindium is 84.2%.
Embodiment 9
A method of purification for ethyl dimethyl indium, comprises the following steps:
1. title complex replacement(metathesis)reaction: under nitrogen protection, tri-n-octyl phosphine is added in reactor, then add ethyl dimethyl indium and etherate (mol ratio of ethyl dimethyl indium and etherate, tri-n-octyl phosphine is 1:1.2) under agitation, continue stirring and carry out replacement(metathesis)reaction in 2 hours;
2. ethers reclaims: at vacuum tightness 380mmHg, temperature 90 DEG C, distill the ether that 10h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 4 ~ 20 removing ether and lower-boiling impurities at vacuum tightness 50mmHg, temperature 80 DEG C;
4. solution is joined: at vacuum tightness 80mmHg, temperature 210 DEG C, solution joins acquisition ethyl dimethyl indium crude product;
5. rectifying: ethyl dimethyl indium crude product is sent into rectifying tower rectifying and obtains high-purity ethyl dimethyl indium (purity >=99.9999%), the pressure of rectifying tower is 320mmHg, column bottom temperature 155 DEG C, reflux ratio 13:1; Wherein, rectifying tower adopts packing tower, and the filler of packing tower adopts the loose filler of heap, and the loose filler of heap is ring-type, is of a size of 3mm ~ 50mm; The theoretical plate number of packing tower is 35.
In the present embodiment, the yield of ethyl dimethyl indium is 85.7%.
Claims (6)
1. a method of purification for alkyl indium, is characterized in that, comprises the following steps:
1. title complex replacement(metathesis)reaction: under protection of inert gas, adds phosphine class part in reactor, then adds alkyl indium and ethers title complex under agitation, continues stirring and carries out replacement(metathesis)reaction in 1 ~ 5 hour;
2. ethers reclaims: at vacuum tightness 100 ~ 600mmHg, temperature 60 ~ 120 DEG C, distill the ethers that 5 ~ 15h recovery replacement(metathesis)reaction displaces;
3. removal of impurities: distill 4 ~ 20h and remove ether and lower-boiling impurity at vacuum tightness 1 ~ 100mmHg, temperature 60 ~ 120 DEG C;
4. solution is joined: at vacuum tightness 1 ~ 100mmHg, temperature 100 ~ 220 DEG C, solution joins acquisition alkyl indium crude product;
5. rectifying: alkyl indium crude product is sent into rectifying tower rectifying and obtains high-purity alkyl indium.
2. the method for purification of alkyl indium as claimed in claim 1, is characterized in that, the mol ratio of described alkyl indium and ethers title complex, phosphine class part is 1:1 ~ 3.
3. the method for purification of alkyl indium as claimed in claim 1, it is characterized in that, described phosphine class part is triphenylphosphine or alkylphosphines; Wherein, the alkyl in alkylphosphines is the alkyl of C atomicity 4-8.
4. the method for purification of alkyl indium as claimed in claim 1, is characterized in that, the ethers in described alkyl indium and ethers title complex is ether or tetrahydrofuran (THF).
5. the method for purification of alkyl indium as claimed in claim 1, is characterized in that, step 5. described in the pressure of rectifying tower be 200 ~ 500mmHg, column bottom temperature 100 ~ 160 DEG C, reflux ratio 5 ~ 20:1.
6. the method for purification of alkyl indium as claimed in claim 1, is characterized in that, described step 5. in rectifying tower used be packing tower.
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| CN201510798429.4A CN105254654A (en) | 2015-11-19 | 2015-11-19 | Method for purifying alkyl indium |
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| CN201510798429.4A CN105254654A (en) | 2015-11-19 | 2015-11-19 | Method for purifying alkyl indium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879900A (en) * | 2018-12-18 | 2019-06-14 | 安徽亚格盛电子新材料有限公司 | A method of trimethyl aluminium is effectively purified using inorganic salts |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62185090A (en) * | 1986-02-10 | 1987-08-13 | Sumitomo Chem Co Ltd | Purification of alkylgallium |
| CN102718784A (en) * | 2012-07-05 | 2012-10-10 | 广东先导稀材股份有限公司 | Decomplexation method of metal organic compound and ether complex |
| CN103145745A (en) * | 2013-03-06 | 2013-06-12 | 江苏南大光电材料股份有限公司 | Method for industrially preparing high-purity metal organic compound |
-
2015
- 2015-11-19 CN CN201510798429.4A patent/CN105254654A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62185090A (en) * | 1986-02-10 | 1987-08-13 | Sumitomo Chem Co Ltd | Purification of alkylgallium |
| CN102718784A (en) * | 2012-07-05 | 2012-10-10 | 广东先导稀材股份有限公司 | Decomplexation method of metal organic compound and ether complex |
| CN103145745A (en) * | 2013-03-06 | 2013-06-12 | 江苏南大光电材料股份有限公司 | Method for industrially preparing high-purity metal organic compound |
Non-Patent Citations (2)
| Title |
|---|
| ANTHONY C. JONES等: "Electrochemical Studies of Group 3 Alkyl Derivatives. Part 1 Synthesis of Trimethylgallium Adducts", 《J. CHEM. SOC. DALTON TRANS》 * |
| 黄柏标等: "制备和提纯三甲基镓（TMG）的新方法", 《人工晶体学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879900A (en) * | 2018-12-18 | 2019-06-14 | 安徽亚格盛电子新材料有限公司 | A method of trimethyl aluminium is effectively purified using inorganic salts |
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