CN101479220A - Process for producing high-purity hexafluoropropylene and cleaning gas - Google Patents
Process for producing high-purity hexafluoropropylene and cleaning gas Download PDFInfo
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- CN101479220A CN101479220A CNA2007800242140A CN200780024214A CN101479220A CN 101479220 A CN101479220 A CN 101479220A CN A2007800242140 A CNA2007800242140 A CN A2007800242140A CN 200780024214 A CN200780024214 A CN 200780024214A CN 101479220 A CN101479220 A CN 101479220A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
Abstract
A process for industrially advantageously producing high-purity hexafluoropropylene; and a use of this high-purity hexafluoropropylene, specifically, a cleaning gas for removing deposits in a semiconductor manufacturing apparatus or liquid-crystal manufacturing apparatus. In the process for high-purity hexafluoropropylene production, crude hexafluoropropylene produced by the pyrolysis of chlorodifluoromethane is purified to thereby produce high-purity hexafluoropropylene. It comprises: a step (1) in which the crude hexafluoropropylene is brought into contact with an adsorbent comprising a zeolite having an average micropore diameter of 3.4-11 AA and/or a carbonaceous adsorbent having an average micropore diameter of 3.5-11 AA to reduce the content of chlorine compounds and/or hydrocarbons in the crude hexafluoropropylene; and a step (2) in which the hexafluoropropylene obtained in the step (1) is distilled to reduce the content of low-boiling ingredients therein.
Description
Technical field
The present invention relates to the manufacture method of high purity R 1216.Particularly, relate to and to be used to remove in the semiconductor-fabricating device ideally or the manufacture method of the sedimental R 1216 in the liquid crystal manufacturing installation and the purposes of high purity R 1216.
Background technology
R 1216 (below be sometimes referred to as " CF
3CF=CF
2" or " FC-1216 ") purgative gas, octafluoropropane (C in semiconducter device manufacturing process for example
3F
8) production of raw material for use etc. in use.As its manufacture method, people know for example following method:
(1) shown in the following formula via chlorodifluoromethane (CHClF
2) thermolysis and make tetrafluoroethylene (CF
2=CF
2) operation in the method that obtains as by product,
2CHClF
2+H
2O→CF
2＝CF
2+CF
3CF＝CF
2
(2), or tetrafluoroethylene the method that obtains such as passed through under decompression, high temperature on platinum by with the tetrafluoroethylene thermolysis,
(3) the non-ring type hydro carbons of the halogenated C3 of propane, propylene or part is carried out the method (spy opens flat 4-145033 communique) of chlorofluorination and dehalogenation,
Or the like, but in most cases, contain various impurity such as saturated compound, unsaturated compound such as Chlorofluorocarbons (CFCs) (CFC) class, Hydrochlorofluorocarbons (HCFC) class, hydrocarbon (HC) class in the R 1216.These impurity are difficult to separate with R 1216 by distillation procedure.
So,, must remove these impurity in order to obtain the higher R 1216 of purity as far as possible.Particularly, for chloro-fluoro-carbon kind, Hydrochlorofluorocarbons class as chlorine-containing compound, except purpose with the R 1216 high purityization, from preventing viewpoints such as ozonosphere is destroyed, preventing in the semiconductor-fabricating device or liquid crystal manufacturing installation internal contamination viewpoints such as (being polluted by chlorine-containing compound in the etching chamber), common distillation must be difficult to isolated compound and also remove.
But, among described impurity, also have owing to form azeotropic mixture or azeotrope-like mixture, so separate the very compound of difficulty with R 1216 with R 1216.For example, chlorine vinyl fluoride (CH
2=CClF), chlorotrifluoroethylene (CF
2=CClF), Refrigerant 12 (CCl
2F
2) etc., because they and R 1216 boiling point are approaching, and form azeotropic mixture or azeotrope-like mixture, so be the very compound of difficulty of separation and purification.
Important compound as heat-eliminating medium is 1,1,1,2-Tetrafluoroethane (CF
3CH
2F), pentafluoride ethane (CF
3CHF
2) etc., as the method for its purifying impurity, people know for example following method: utilize extractive distillation to carry out the method for purifying; Dehalogenation hydrogenation by using hydrogen in the presence of catalyzer etc. is removed the method for impurity.
In addition, the nitrogen trifluoride (NF in order to use as purgative gas
3), hexafluoroethane (CF
3CF
3) wait the saturated compound high purityization, also in order to reduce this chlorine-containing compound (purifying), people propose and have implemented the whole bag of tricks, thereby realize high purityization.
On the other hand, as the method for using R 1216 as purgative gas, people for example know,
(1) plasma CVD reaction chamber cleaning method and plasma-etching method (spy opens flat 9-296271 communique),
(2) etching gas and purgative gas (spy opens flat 10-27781 communique),
(3) purging method and the substrate board treatment (spy opens the 2005-26409 communique) in the treatment chamber,
Or the like, but about the impurity in the R 1216, particularly about purification process, high purityization, still leave problem and problem as the chlorine-containing compound of source of pollution.
Patent documentation 1: the spy opens flat 4-145033 communique
Patent documentation 2: the spy opens flat 9-296271 communique
Patent documentation 3: the spy opens flat 10-27781 communique
Patent documentation 4: the spy opens the 2005-26409 communique
Summary of the invention
The present invention will solve the problem that above-mentioned prior art exists, its objective is the favourable industrially preparing process that the high purity R 1216 is provided, and provide the purposes of this high purity R 1216, specifically, its objective is and be provided for removing in the semiconductor-fabricating device or the sedimental purgative gas in the liquid crystal manufacturing installation.
Present inventors further investigate in order to address the above problem, found that, combination by following operation can obtain highly purified R 1216, thereby finish the present invention, described operation is that to make the described thick R 1216 that contains chlorine-containing compound and/or hydro carbons be 3.4 with containing average fine pore
～11
Zeolite and/or average fine pore be 3.5
～11
The sorbent material contact of carbonaceous adsorbent, thereby reduce the operation and the distillation purifying operation of the content of chlorine-containing compound and/or hydro carbons.
That is, the present invention is made of following [1]～[15].
[11] a kind of manufacture method of high purity R 1216 is that the thick R 1216 that will make via the chlorodifluoromethane thermolysis carries out purifying, thereby makes the method for high purity R 1216, comprises following operation (1) and operation (2),
Operation (1): making described thick R 1216 is 3.4 with containing average fine pore
～11
Zeolite and/or average fine pore be 3.5
～11
The sorbent material contact of carbonaceous adsorbent, thereby reduce the chlorine-containing compound in the thick R 1216 and/or the content of hydro carbons;
Operation (2): by distilling the content of the low boiling point component in the R 1216 that reduces operation (1) gained.
[2] according to the manufacture method of above-mentioned [1] described high purity R 1216, described chlorine-containing compound is general formula C
vH
xCl
yF
zAt least a kind of shown compound, in the above-mentioned general formula, v is 1～4 integer, and x is 0～2 integer, and y is 1～3 integer, and z is 1～6 integer, 2v ≦ x+y+z ≦ 2v+2.
[3] according to the manufacture method of above-mentioned [1] described high purity R 1216, described chlorine-containing compound is at least a kind that is selected from Refrigerant 12, Dichloromonofluoromethane, chlorodifluoromethane, chlorine vinyl fluoride, chlorotrifluoroethylene, chloro-tetrafluoroethane, chloropentafluoroethane and the chlorine HFC-236fa.
[4] according to the manufacture method of above-mentioned [1] described high purity R 1216, described hydro carbons is at least a kind that is selected from propylene, cyclopropane and the propane.
[5] according to the manufacture method of above-mentioned [1] described high purity R 1216, described zeolite is that the ratio of silicon-dioxide/aluminium is the zeolite below 2.0.
[6] according to the manufacture method of above-mentioned [1] described high purity R 1216, described low boiling point component is to be selected from least a in nitrogen, oxygen, carbon monoxide and the carbonic acid gas.
[7] according to the manufacture method of above-mentioned [1] described high purity R 1216, the thick R 1216 that will make via the chlorodifluoromethane thermolysis distills, thereby reduces the high boiling point component content in the thick R 1216, supplies with described operation (1) then.
[8] according to the manufacture method of above-mentioned [1] described high purity R 1216, the chlorine-containing compound content by volume in the high purity R 1216 of described operation (2) gained is below the 20ppm.
[9] according to the manufacture method of above-mentioned [1] described high purity R 1216, the hydrocarbon content by volume in the high purity R 1216 of described operation (2) gained is below the 30ppm.
[10] according to the manufacture method of above-mentioned [1] described high purity R 1216, the content by volume of the low boiling point component in the high purity R 1216 of described operation (2) gained is below the 20ppm.
[11] according to the manufacture method of above-mentioned [1] described high purity R 1216, the purity of the high purity R 1216 of described operation (2) gained is more than the 99.99 volume %.
[12] according to the manufacture method of above-mentioned [1] described high purity R 1216, described high purity R 1216 uses as being used to remove semiconductor-fabricating device sedimental purgative gas interior or that the liquid crystal manufacturing installation is interior.
[13] a kind of sedimental purgative gas that is used to remove in semi-conductor or the liquid crystal manufacturing installation is that chlorine-containing compound content by volume is that 20ppm is following, the hydrocarbon content by volume is that 30ppm is following and low boiling point component content by volume is below the 20ppm and purity is the above high purity R 1216s of 99.99 volume %.
[14] according to above-mentioned [13] described purgative gas, described high purity R 1216 is to use each the high purity R 1216 of method manufacturing of above-mentioned [1]～[12].
[15] a kind of purging method uses above-mentioned [13] described purgative gas, under the pressure of the temperature of 50～500 ℃ of scopes, 0.05～1MPa scope, removes in the semiconductor-fabricating device or the settling in the liquid crystal manufacturing installation.
By the present invention, can be with easy method, make highly purified R 1216 effectively, and can use the high purity R 1216 that obtains ideally as being used to remove in the semiconductor-fabricating device or the sedimental plasma clean gas in the liquid crystal manufacturing installation.
Embodiment
Below, optimal way of the present invention is elaborated.
The manufacture method of high purity R 1216 of the present invention is to make the method for high purity R 1216 by the thick R 1216 of purifying.Specifically, comprise following operation (1) and operation (2): (1) makes above-mentioned thick R 1216 is 3.4 with containing average fine pore
～11
Zeolite and/or average fine pore be 3.5
～11
The sorbent material contact of carbonaceous adsorbent, thereby reduce the operation of the content of chlorine-containing compound in the thick R 1216 and/or hydro carbons; (2) by distilling the operation of the low boiling point component content in the R 1216 that reduces above-mentioned operation (1) gained.
Thick R 1216 used in the present invention is made as by product when making tetrafluoroethylene via the chlorodifluoromethane thermolysis, contains the various impurity such as saturated compound, unsaturated compound of chlorine-containing compound, hydrogen fluorohydrocarbon (HFC) class, hydrocarbon (HC) classes etc. such as Chlorofluorocarbons (CFCs) (CFC) class.
As above-mentioned chlorine-containing compound, can enumerate general formula C
vH
xCl
yF
z(in the formula, v is 1～4 integer, and x is 0～2 integer, and y is 1～3 integer, and z is 1～6 integer, and compound shown in 2v ≦ x+y+z ≦ 2v+2) contains these compounds more than a kind or 2 kinds in the thick R 1216.As the concrete example of compound shown in the above-mentioned general formula, can enumerate Refrigerant 12 (CCl
2F
2), Dichloromonofluoromethane (CHCl
2F), chlorodifluoromethane (CHClF
2), chlorine vinyl fluoride (CH
2=CClF), chlorotrifluoroethylene (CF
2=CClF), chloro-tetrafluoroethane (CF
3CHClF), chloropentafluoroethane (CF
3CClF
2) and chlorine HFC-236fa (CF
3CHFCClF
2) etc.The content of above-mentioned chlorine-containing compound is preferably below the 0.05 volume % in the thick R 1216.
As above-mentioned hydrogen fluorohydrocarbon class, can enumerate difluoroethylene (CHF=CHF), Tetrafluoroethane (CF
3CH
2F), trifluoro propene (CF
3CH=CH
2), fluorine propylene (CH
3CF=CH
2) etc.The content of above-mentioned hydrogen fluorohydrocarbon class is preferably below the 0.05 volume % in the thick R 1216.
As above-mentioned hydro carbons, can enumerate propylene (CH
2=CHCH
3), cyclopropane (C
3H
6), propane (CH
3CH
2CH
3) etc.The content of above-mentioned hydro carbons is preferably below the 0.05 volume % in the thick R 1216.
Sorbent material used in the present invention is that (1) average fine pore is 3.4
～11
Zeolite, (2) average fine pore be 3.5
～11
Carbonaceous adsorbent or the mixture of (3) above-mentioned zeolite and above-mentioned carbonaceous adsorbent.Average fine pore is the effect excellence that the zeolite of above-mentioned scope reduces the foreign matter content in the thick R 1216.In addition, average fine pore is the effect excellence that the carbonaceous adsorbent of above-mentioned scope reduces the foreign matter content in the thick R 1216.And then from the viewpoint of the reduction effect that further improves foreign matter content, more preferably the ratio of silicon-dioxide/aluminium is the zeolite below 2.0.
That is, the employed zeolite of the manufacture method of high purity R 1216 of the present invention preferably has
More preferably
The zeolite of average fine pore.If average fine pore greater than
Zeolite, then the adsorptive capacity of R 1216 increases sometimes, if average fine pore less than
Zeolite, the ability of then adsorbing chlorine-containing compound, hydro carbons sometimes reduces.
In addition, the ratio of the Si of preferred zeolite (silicon-dioxide)/Al (aluminium) is below 2.0, the ratio of Si/Al greater than 2 situation under, can not optionally adsorb chlorine-containing compound, hydro carbons sometimes.As zeolite, be preferably selected from molecular sieve 4A (MS-4A, the manufacturing of ユ ニ オ Application Showa Corporation), molecular sieve 5A (MS-5A, the manufacturing of ユ ニ オ Application Showa Corporation), molecular sieve 10X (MS-10A, ユ ニ オ Application Showa Corporation makes) and at least a zeolite of molecular sieve 13X (MS-13X, the manufacturing of ユ ニ オ Application Showa Corporation).
On the other hand, as carbonaceous adsorbent, known have activated carbon, a carbonaceous molecular sieve.Activated carbon is to be raw material with Exocarpium cocois (Cocos nucifera L), coal, timber etc., thereby after high temperature cabonization, make raw material generate the special processing activatory carbon that tax is lived that is called of pore, its sorbent material as excellence has purposes widely, but in manufacture method of the present invention, the preferred carbonaceous molecular sieve that uses the molecular sieve activated carbon of highly being controlled as fine pore.
Carbonaceous adsorbent preferably has
The sorbent material of average fine pore, if average fine pore greater than
Carbonaceous adsorbent, then the adsorptive capacity of R 1216 increases sometimes, if average fine pore less than
Carbonaceous adsorbent, the ability of then adsorbing chlorine-containing compound, hydro carbons sometimes reduces.As carbonaceous adsorbent, preferred carbonaceous molecular sieve 4A (for example Takede Chemical Industries Ltd makes) or carbonaceous molecular sieve 5A (for example Takede Chemical Industries Ltd makes), they also can and be used.
In addition, in containing the above-mentioned sorbent material of above-mentioned zeolite and carbonaceous adsorbent,, can suitably set according to kind, the content of impurity in the thick R 1216 to the not restriction especially of ratio of mixture of zeolite and carbonaceous adsorbent.
As mentioned above, in the present invention, contact with thick R 1216, reduce the content of chlorine-containing compound and/or hydro carbons by making above-mentioned sorbent material.Not restriction especially of the state of thick R 1216 when sorbent material is contacted with thick R 1216, for example can be to make thick R 1216 with the method for gaseous phase contact, with the method for gas-liquid mixed state contact or with the arbitrary method in the method for liquid state contact, but it is the method efficient with the liquid state contact is good, so preferred.
To the contact method of sorbent material with thick R 1216, not restriction especially, but for example can use known method such as batch-type, continous way.Industrial for example generally is, 2 fixed-bed type adsorption towers are set, if one to reach absorption saturated then it is changed and the regenerated method.In addition, to the not restriction especially of condition of contact position reason, but the preferred low temperature of treatment temp, for example, preferred-50～50 ℃ temperature range, more preferably-20～30 ℃ temperature range.In addition, under the situation that makes thick R 1216 with the liquid state contact, processing pressure is so long as can keep the pressure of liquid state to get final product, not restriction especially, in addition, to also restriction especially of situation, but be preferably the scope of 0.05MPa～1MPa with gaseous phase contact.
Described thick R 1216 also can be with before described sorbent material contacts, import distillation tower in advance and remove low boiling point component (low boiler cut), high boiling point composition (high boiling fraction), but in this case, the low boiling point component of self-absorbent might be sneaked into, low boiling point component must be removed once more.So, in manufacture method involved in the present invention, after (1) makes described thick R 1216 and described sorbent material contacts, implement (2) and the R 1216 of this operation (1) gained distilled and the operation that reduces the content of low boiling point component.In addition, preferably reduce high boiling point composition in the thick R 1216 before in advance in above-mentioned contact operation (1), preferably have operation in the present invention, that is: in above-mentioned contact operation (1) thus before thick R 1216 is distilled the content of the high boiling point composition that reduces in the thick R 1216.
As above-mentioned low boiling point component, can enumerate nitrogen, oxygen, carbon monoxide, carbonic acid gas and the mixture more than 2 kinds in them.
So, after making thick R 1216 and above-mentioned sorbent material contacts, can reduce the content of chlorine-containing compound, hydro carbons, low boiling point component by distillation, be the above high purity R 1216s of 99.99 volume % thereby can obtain purity.The content by volume of chlorine-containing compound is preferably below the 20ppm in this high purity R 1216, more preferably by volume is below the 10ppm, the preferred by volume of the content of hydro carbons is below the 30ppm, by volume is more preferably below the 20ppm, the preferred by volume of the content of low boiling point component is below the 20ppm, and more preferably by volume is below the 10ppm.
Such high purity R 1216 can be used as the sedimental purgative gas use that is used to remove in the semiconductor-fabricating device or in the liquid crystal manufacturing installation.At this moment, both can use the high purity R 1216 separately, also can add being selected from He, Ar, N according to cleaning condition
2, at least a kind of carrier gas in Ne, Kr, the oxygenatedchemicals.As above-mentioned oxygenatedchemicals, can enumerate O
2, CO, CO
2, NO, N
2O, OF
2, COF
2Deng.The addition of these diluent gass is preferably below the 40 volume %.
State in the use under the situation that purgative gas cleans semiconductor-fabricating device, both can under condition of plasma, clean, also can under no condition of plasma, clean.Under the situation of under condition of plasma, cleaning, as long as excitaton source can inspire plasma body from above-mentioned purgative gas, restriction especially, if but use the microwave-excitation source then cleaning efficiency is good, so preferred.In addition, use the temperature range of purgative gas of the present invention, pressure range to get final product not restriction especially, but the temperature of preferred 50～500 ℃ of scopes, the pressure of preferred 0.05～1MPa scope so long as can generate the scope of plasma body.On the other hand, in the situation of under no condition of plasma, cleaning, it is indoor that purgative gas is imported case, preferably that case is indoor pressure is set at the scope of 0.05～1MPa, activate purgative gas by at least a portion of case is indoor and purgative gas or the scope that the either party is heated to 150～500 ℃, thereby can the settling etching be removed by having accumulated sedimental zone, clean semiconductor-fabricating device from case chamber and other.
Embodiment
Below, by embodiment the present invention is described, but the present invention is not subjected to any restriction of these embodiment.
Preparation example 1
Via thermolysis (600 ℃ of heat decomposition temperatures) from chlorodifluoromethane (CHClF
2) when making tetrafluoroethylene, resultant is carried out 2 distillations and reclaims tetrafluoroethylene, obtain thick R 1216 then.Analyze this thick R 1216 with gas-chromatography [(strain) Shimadzu Seisakusho Ltd. makes " GC-14A ", post: (strain) Shimadzu Seisakusho Ltd. makes Porapack-Q (6m), measures temperature: 80～200 ℃], show the result in table 1.
Embodiment 1
(ユ ニ オ Application Showa Corporation makes: average fine pore 10 with 80g molecular sieve 13X
, ratio=0.81 of silicon-dioxide/aluminium) and (carbonaceous molecular sieve 5A, Takede Chemical Industries Ltd makes: average fine pore with the 70g carbonaceous adsorbent
) mix and be filled in the stainless steel rounding tube of volume 1000ml, carry out vacuum-drying.Then, on one side cylinder is cooled off, to the thick R 1216 of wherein filling above-mentioned preparation example 1 gained of about 550g, at room temperature stir often on one side, fill and reclaim liquid phase part [operation (1)] after about 12 hours.Analyze this liquid phase part with gas-chromatography [(strain) Shimadzu Seisakusho Ltd. makes " GC-14A ", post: (strain) Shimadzu Seisakusho Ltd. makes Porapack-Q (6m), measures temperature: 80～200 ℃].Show the result in table 1.
Then, with the liquid phase part importing distillation tower of above-mentioned operation (1) gained, the top of tower taking-up low boiling point component (low boiler cut) from distillation tower reclaims liquid phase part [operation (2)] from the bottom of distillation tower.Analyze this liquid phase part with gas-chromatography [(strain) Shimadzu Seisakusho Ltd. makes " GC-14A ", post: (strain) Shimadzu Seisakusho Ltd. makes Porapack-Q (6m), measures temperature: 80～200 ℃].Show the result in table 1.
Reference example 1
(ユ ニ オ Application Showa Corporation makes: average fine pore 10 with 30g molecular sieve 13X
, silicon-dioxide/aluminium ratio=0.81) be filled in the stainless steel rounding tube of volume 200ml, carry out vacuum-drying.Then,, to the thick R 1216 of wherein filling above-mentioned preparation example 1 gained of about 70g, at room temperature stir often on one side, fill after about 12 hours and reclaim liquid phase part on one side with the cylinder cooling.Analyze this liquid phase part with gas-chromatography [(strain) Shimadzu Seisakusho Ltd. makes " GC-14A ", post: (strain) Shimadzu Seisakusho Ltd. makes Porapack-Q (6m), measures temperature: 80～200 ℃].Show the result in table 1.
Reference example 2
(carbonaceous molecular sieve 5A, Takede Chemical Industries Ltd makes: average fine pore 5 with the 20g carbonaceous adsorbent
) be filled in the stainless steel rounding tube of volume 200ml, carry out vacuum-drying.Then, on one side cylinder is cooled off, to the thick R 1216 of wherein filling above-mentioned preparation example 1 gained of about 60g, at room temperature stir often on one side, fill after about 12 hours and reclaim liquid phase part.Analyze this liquid phase part with gas-chromatography [(strain) Shimadzu Seisakusho Ltd. makes " GC-14A ", post: (strain) Shimadzu Seisakusho Ltd. makes Porapack-Q (6m), measures temperature: 80～200 ℃].Show the result in table 1.
[table 1]
(unit: volume %)
Claims (15)
1. the manufacture method of a high purity R 1216 is that the thick R 1216 that will produce via the chlorodifluoromethane thermolysis carries out purifying, thereby makes the method for high purity R 1216, comprises following operation (1) and operation (2),
Operation (1): making described thick R 1216 is 3.4 with containing average fine pore
～11
Zeolite and/or average fine pore be 3.5
～11
The sorbent material contact of carbonaceous adsorbent, thereby reduce the chlorine-containing compound in the thick R 1216 and/or the content of hydro carbons;
Operation (2): by distilling the content of the low boiling point component in the R 1216 that reduces operation (1) gained.
2. the manufacture method of high purity R 1216 according to claim 1, described chlorine-containing compound are general formula C
vH
xCl
yF
zAt least a kind of shown compound, in the above-mentioned general formula, v is 1～4 integer, and x is 0～2 integer, and y is 1～3 integer, and z is 1～6 integer, 2v≤x+y+z≤2v+2.
3. the manufacture method of high purity R 1216 according to claim 1, described chlorine-containing compound are at least a kind that is selected from Refrigerant 12, Dichloromonofluoromethane, chlorodifluoromethane, chlorine vinyl fluoride, chlorotrifluoroethylene, chloro-tetrafluoroethane, chloropentafluoroethane and the chlorine HFC-236fa.
4. the manufacture method of high purity R 1216 according to claim 1, described hydro carbons are at least a kind that is selected from propylene, cyclopropane and the propane.
5. the manufacture method of high purity R 1216 according to claim 1, described zeolite are that the ratio of silicon-dioxide/aluminium is the zeolite below 2.0.
6. the manufacture method of high purity R 1216 according to claim 1, described low boiling point component are to be selected from least a in nitrogen, oxygen, carbon monoxide and the carbonic acid gas.
7. the manufacture method of high purity R 1216 according to claim 1, the thick R 1216 that will produce via the chlorodifluoromethane thermolysis distills, thereby reduces the high boiling point component content in the thick R 1216, is supplied to described operation (1) then.
8. the manufacture method of high purity R 1216 according to claim 1, the chlorine-containing compound content by volume in the high purity R 1216 of described operation (2) gained is below the 20ppm.
9. the manufacture method of high purity R 1216 according to claim 1, the hydrocarbon content by volume in the high purity R 1216 of described operation (2) gained is below the 30ppm.
10. the manufacture method of high purity R 1216 according to claim 1, the content by volume of the low boiling point component in the high purity R 1216 of described operation (2) gained is below the 20ppm.
11. the manufacture method of high purity R 1216 according to claim 1, the purity of the high purity R 1216 of described operation (2) gained is more than the 99.99 volume %.
12. the manufacture method of high purity R 1216 according to claim 1, described high purity R 1216 uses as being used to remove semiconductor-fabricating device sedimental purgative gas interior or that the liquid crystal manufacturing installation is interior.
13. a sedimental purgative gas that is used to remove in semi-conductor or the liquid crystal manufacturing installation is that chlorine-containing compound content by volume is that 20ppm is following, the hydrocarbon content by volume is that 30ppm is following and low boiling point component content by volume is below the 20ppm and purity is the above high purity R 1216s of 99.99 volume %.
14. purgative gas according to claim 13, described high purity R 1216 are to use each the high purity R 1216 of method manufacturing of claim 1～12.
15. a purging method uses the described purgative gas of claim 13, under the pressure of the temperature of 50～500 ℃ of scopes, 0.05～1MPa scope, removes in the semiconductor-fabricating device or the settling in the liquid crystal manufacturing installation.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| JP181477/2006 | 2006-06-30 | ||
| JP2006181477 | 2006-06-30 |
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| CN101479220A true CN101479220A (en) | 2009-07-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2007800242140A Pending CN101479220A (en) | 2006-06-30 | 2007-06-28 | Process for producing high-purity hexafluoropropylene and cleaning gas |
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| Country | Link |
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| JP (1) | JP5132555B2 (en) |
| CN (1) | CN101479220A (en) |
| WO (1) | WO2008001844A1 (en) |
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| CN102695692A (en) * | 2009-10-15 | 2012-09-26 | 墨西哥化学阿玛科股份有限公司 | Process for purifying (hydro) fluoroalkenes |
| CN102766016A (en) * | 2012-08-09 | 2012-11-07 | 山东东岳高分子材料有限公司 | Method for recovering octafluoropropane from hexafluoropropylene production process |
| CN104788283A (en) * | 2015-03-12 | 2015-07-22 | 福建三农化学农药有限责任公司 | Double line rectification method of hexafluoropropene production cracking gas, and rectification apparatus thereof |
| CN113784776A (en) * | 2019-08-06 | 2021-12-10 | 昭和电工株式会社 | Gas processing method and gas processing apparatus |
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| FR2933402B1 (en) | 2008-07-03 | 2010-07-30 | Arkema France | PROCESS FOR PURIFYING 2,3,3,3-TETRAFLUORO-1-PROPENE (HFO1234YF) |
| TW201103972A (en) | 2009-04-01 | 2011-02-01 | Solvay Fluor Gmbh | Process for the manufacture of etched items |
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| AU2013204796B2 (en) * | 2009-10-15 | 2014-09-11 | Mexichem Amanco Holding S.A. De C.V. | Process for purifying (hydro) fluoroalkenes |
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| JPS51128901A (en) * | 1975-05-02 | 1976-11-10 | Daikin Ind Ltd | Separation method |
| GB8708618D0 (en) * | 1987-04-10 | 1987-05-13 | Ici Plc | Production process |
| JP2542394B2 (en) * | 1987-08-06 | 1996-10-09 | イー・アイ・デユポン・ドウ・ヌムール・アンド・カンパニー | Hexafluoropropylene purification method |
| JPH09296271A (en) * | 1996-05-02 | 1997-11-18 | Samuko Internatl Kenkyusho:Kk | Method for cleaning plasma cvd reaction chamber and plasma etching method |
| JPH1027781A (en) * | 1996-07-10 | 1998-01-27 | Daikin Ind Ltd | Etching gas and cleaning gas |
| JP4220318B2 (en) * | 2003-07-01 | 2009-02-04 | 大陽日酸株式会社 | Cleaning method inside process chamber |
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- 2007-06-28 JP JP2008522621A patent/JP5132555B2/en not_active Expired - Fee Related
- 2007-06-28 CN CNA2007800242140A patent/CN101479220A/en active Pending
- 2007-06-28 WO PCT/JP2007/062995 patent/WO2008001844A1/en active Application Filing
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| CN104788283A (en) * | 2015-03-12 | 2015-07-22 | 福建三农化学农药有限责任公司 | Double line rectification method of hexafluoropropene production cracking gas, and rectification apparatus thereof |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP5132555B2 (en) | 2013-01-30 |
| JPWO2008001844A1 (en) | 2009-11-26 |
| WO2008001844A1 (en) | 2008-01-03 |
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