Process for preparing polyfluorocarbon

专利摘要:
A novel chemical compound poly-dicarbon monofluoride represented by the formula (C2F)n and having a crystalline structure of packing form featured by its layer structure as shown in FIG. 12 hereof stacked with an interlayer spacing of about 9.0 A. Such new compound can be produced under relatively mild reaction conditions and obtained in a yield as large as 100% with respect to not only the carbon material employed but also the fluorine employed. The new compound is black under the formation conditions and of low crystallinity, but it can be easily converted to that of high crystallinity and white color by heat treatment in a fluorine atmosphere. The new compound has a wide variety of uses, for example, as lubricants, stain-resistant and water-repellent materials, cathode materials in high energy primary cells, etc.
公开号:SU1058502A3
申请号:SU782573700
申请日:1978-02-03
公开日:1983-11-30
发明作者:Ватанабе Нобуацу；Кита Ясуси
申请人:Эпплайд Сайенс Рисерч Институт (Фирма)；Ватанабе Нобуацу；
IPC主号:

专利说明:

The invention relates to the technology of carbon compounds with fluorine, in part to a process for the preparation of the chemical compound pLidicarbonmonofluoride, described by the formula, which can be used as a cathode material in high energy galvanic cells. Closest to the present invention is a method for producing a polyfluorocarbon, which includes the repeated treatment of carbon-containing material (artificial graphite in the form of products or pieces) with fluorine gas at 200–1000 ° C under reduced pressure. According to this method, polyfluorocarbons (CPs) are obtained mainly, namely (CPX), 0, which has a crystalline structure, in which the structural layers are located approximately 5, 8A 1 apart from each other. The disadvantages of the known method are the instability of the polyfluorocarbon of this formula and the low yield (only a few percent regarding the amount of south fluorine used and a few tens of percent relative to the amount of carbon-containing material used). Compounds (CPs) have valuable properties, but because of the difficulty of their production, industrial use (CPs) is extremely limited due to their high cost. The purpose of the invention is to increase the yield of a polyfluorocarbon of the formula (having a complex of valuable properties comparable or superior to those of a lower cost, simplifying the process, as well as increasing the crystal personality of the resulting product. This goal is achieved by the method of producing a polyfluorocarbon Carbonaceous material with Franklin parameter up to 0.6 and particle size from 1 to 150 microns and processing are used for the treatment of carbon-containing material, with fluorine gas at 300-500 0. with fluorine-containing gases is carried out until a constant weight of the material is reached. The treatment is carried out at a pressure of fluorine gas of 50 mm Hg, up to 1.5 atm, within 0.6-150 hours. Natural graphite or graphite coke is used as carbon-containing material. The material is further subjected to heat treatment up to 600 ° C in an atmosphere of gaseous I fluorine for 5–120 h at a pressure of the research institute not less than 50 NM Hg. According to the proposed method, chemical compounds of prlidicarbonmonofluorides of stoichiometric formula (, 10–10, having The architectural structure, the distance between the intermediates and the layers, is approximately 9.0 AJ yield up to 100% relative to not only the carbon-containing material, but also the amount of fluorine used, and the preparation process is simplified by eliminating multiple fluoride treatments. Figure 1 is a diagram depicting the layered structure of known compounds (CFj, where fluorine atoms A and B are respectively above and below the carbon network B (CF), the distance between the interlayer layers is about 5.8 A, and the layers themselves Figure 2 shows a plot of the F / C ratios of the products obtained as a result of the reaction of natural graphite (obtained in Madagascar And having a purity greater than 99%), characterized by a particle size of 200 to 250 mesh, with fluorine under fluorine pressure 220 220 mm Hg is based on the reaction temperature used, Fig. 2 is constructed according to Table 1, which shows the relationship between reaction temperatures and the F / C ratios of products (empirical formula.) As can be seen from the data presented in Table. 1, in FIG. 2, as the temperature of the reaction increases, the ratio G / C approaches 1. The product obtained at a relatively low temperature, for example 375 ° C, has an F / C ratio of 0.58 (namely, black color). As soon as the product's P / C ratio reaches 0.58, this assignment does not change for 120 hours when the product is heated at 60 ° C under fluorine atmosphere. Only the color of the product varies from black to white. On fig.Z depicts X-ray patterns of the products obtained in the experiments, the data of which are presented in Table 1.2. Fig. 4 shows a graph of the temperature dependence of the distance between the intermediates and the layers (eZ ooo and polyirins (products calculated on X-ray diffraction of FIG. 3). As can be seen from Figs 3 and 4, the peaks associated with the diffraction (001), shifted to small angles, and the half width also changes as the reaction temperature decreases. The distance between the intermediate layers of the crystal lattice of the product obtained as a result of the reactions at is 5.85 L and corresponds to the distance for (CP) "then Kajj the distance between the intermediate layers of the crista The lysis lattice of the product obtained as a result of the reaction at 375 ° C is 9.0 D. The products obtained as a result of reactions proceeding at intermediate temperatures have a distance between the intermediate layers of the crystal lattice of 5.8 9.0 A. Half-width diffraction (OO) increases with increasing Tet-reaction temperature, has maxiglum at a reaction temperature of about 48 ° C, and then decreases with a further increase in reaction temperature in areas within the temperature range of 375-h640 ° C. The resulting products consist mainly of the CijF in the stoichiometric ratio and the CP in the stoichiometric ratio. When diffraction lines (.001) of products obtained as a result of reactions proceeding at 375-640 0 are calculated taking into account the Lorentz deviation coefficient, it becomes obvious that the diffraction lines consist respectively of diffraction lines (C, p) 0 have peak near and at the diffraction lines (CFL, having a peak at 13.5 (20): FIG. 5 shows the X-ray diffraction patterns of the product obtained as a result of the reaction at 120 h and after its processing at 600 ° C for 120 h Fig. 6 shows the X-ray patterns of the product obtained as a result of the reaction at for 6 hours and after its heat treatment at 600 ° C for 22 hours. From Figs. 5 and b it can be seen that both patterns are practically unchanged even after such prolonged heat treatments at such high temperatures. In Fig. 7, E 5 CA-sp kt of the product obtained as a result of the reaction for 48 hours. The spectrum shown in Fig. 7 shows a peak attributed to the CF bond in the CP in stoichiometric communication, with a small shoulder due to the presence of peripheral CP groups, and a small peak associated with the presence of C – C bonds (impurities). In FIG. B, the ESCA spectrum of the product () obtained from the reaction of natural graphite (the same material as described above) with fluorine (200 mm Hg, when at 120 h. From Fig. 8 it can be seen that, in addition to the peak due to the C – H bonds, in the spectrum, peak due to C-C bonds (impurities), there is a shoulder associated with the presence of groups and CFj Avg. and another completely disintegrated shoulder associated with the presence of C – C bonds in the stoichiometric compound Cj F. FIG. 9 represents the E5CA spectrum of the sample obtained from the heat treatment of the product described in fig. 8. As can be seen from FIGS. 8 and 9, practically no difference or change in the shape of the spectrum occurs. This suggests that polydi carbon monofluoride (Cj, p) obtained at relatively low temperature is thermally stable and does not undergo structural changes even during subsequent heat treatment under harsh conditions. FIG. 10 shows the IR spectrum of the product (, CF) obtained by the reaction of 620® C for 48 hours. FIG. 11 shows the IR spectrum of the product (CjF) f, obtained by the reaction at 120 hours). , From FIGS. 10 and 11 it can be seen that there is a noticeable difference between the spectrum (CP) „and the spectrum (CjF). Figure 12 shows the DTA curves of the products obtained respectively by the reaction at 120 h and the reaction at 375 ° C. for 120 hours, and curves for samples obtained by heat treatment of the latter at 600 ° C for 120 hours. FIG. 13 shows the X-ray The programs of products obtained on the basis of carbon-containing materials with different particle sizes of G-diagrams are shown in groups, depending on the reaction temperature T, Fig. 14 shows the X-ray patterns of the products obtained at. different pressures of fluorine gas, (diagrams are shown in groups depending on the reaction temperatures used}. Fig. 15 shows the curve of the increase in weight of the products formed at different reaction temperatures. (The curves were obtained with careful regulation of the fluorine gas inlet and also calculated by empirical for the product characterized by the last curve), FIG. 16 is a diagram of an installation for carrying out the proposed method. The installation consists of an air thermostat (below erzhivayuschego temperature.
round) -1, fan 2, heater 3, nickel prunks 4, covered with teflon of farrit core
5, differential transformer
6, water-cooled shirt 7, shape we are DLI sample (outer diameter
12 mm, 5 km high) 8 of metal, burner 9, nickel reactor 10, thermocouple spa 11, Heusler tubes 12, mercury manometer 13, gas mixing vessel 14, bath 15 with soda lime, bath 16, drexel 17, high pressure vessel 18 for fluorine, linear amplifier 1-9 and recording device 20.
The weight sensitive part is a balanced type spring. The spring 4 is stretched and compressed depending on the change in the weight of the sample, the expansion and compression of the spring 4 is detected by the differential transformer 6. The parts of the apparatus operating at high temperatures are made of nickel and metal, and the parts operating at ambient temperature are of trifluorochloroethane, copper and stainless steel. The spring 4 is made of nickel wire with a diameter of 3 mm, and its diameter is 10, the number of turns is 40, the maximum load is 5 g and the strain is 100 mm / g. The reaction temperature is measured in the part located from the cell for sample 8 at a distance of 0.5 mm using an aluminum-chromal thermocouple placed in the lower part of the reactor 10. The accuracy of temperature control is + 0.5 ° C ...
An important factor determining the formation of polydicarbon monofluoride) s / c in terms of the fluorination of the particulate carbon-containing material is the reaction temperature lying in the range of 300-500 ° C. If the temperature is less than 300 ° C, then the reaction will not proceed. On the other hand, if the reaction temperature exceeds, then the main process is the formation (, CF, then the quantity formed is 1 (CzFJ is small. In addition, at a reaction temperature of 500 ° C, the resulting product tends to decompose, which leads to a significant decrease in yield reactions. Details of this process are discussed below.
The determining factor for obtaining (is also the crystallinity of the crushed carbon-containing material used as the raw material. The carbon-bearing material can be expressed by the parameter of Franklin R.
ranclin P can be calculated on the forum
c5co ") 3g440-0.086 (1-P), where e (oog) is between the intermediate layers {002
To obtain () it is necessary, for example, the parameter of the Franklin P carbon-containing material was in the range of 0-0.6. The carbon-containing material, whose Franklin parameter value is 0., is completely crystalline. For example, the C of such a compound is natural graphite from Madagascar. If the carbonaceous material has a Franklin paragat greater than 0.6, then the pregalling reaction is the formation reaction (CF), and (CjF) He is formed completely. The most preferred material for producing (C2p) is natural graphite. In addition, graphitized carbonaceous materials can be used whose Franklin parameter is less than 0.6 or equal to 0.6, for example, oil cokes that have been heat treated at 2000-30.00 ° C for about 10-120 minutes in a graphitization furnace. .. When using graphitized carbon-containing materials such as petroleum coke, the synthesis products are characterized by a relatively high content of peripheral CP and P groups, since the particle size of petroleum cokes is relatively small
The reaction time is not a determining factor. .
Dp of obtaining () according to the proposed method, it is important that the reaction of the particulate carbon-containing material with fluorine proceeds before the complete fluorination of the first one, i.e. until further heating of the product in a fluorine atmosphere is accompanied by an increase in the fluorine content of this product. The time required for the complete fluorination of the particulate carbon-containing material varies depending on the reaction temperature, the crystallinity of the original carbon-containing material, its particle size and fluorine pressure, but can usually lie in the range from 10 minutes to 150 hours. - Qi fluorination of the particulate carbon-containing material was not completely completed; the final product will contain particles of unreacted carbon-containing matter.
The particle size of the crushed carbon-containing carbon matter is a significant factor. Pain size is too large, it takes too long to complete the fluorination reaction of the carbon-containing material. If the particle size is too small, the process is directed towards the formation (which leads to a decrease in the content of () in the final product. The particle size of the crushed carbon-containing material is selected in the range of 1-150 µm, preferably 30-80, which is confirmed by Fig.13, which shows x-ray products obtained using carbon-containing material with different particle sizes (diagrams are grouped according to the reaction temperatures used. Reaction conditions and the ratio of P / C products, characterized by 13, are presented in Table 2. / As can be seen from the data of Table 2 and Figure 13, the smaller the particle size, the higher the content (Cjf) B of the product, however, if the particle size is too small, for example, smaller than 400 mesh (Tyler) actively take place formation reaction (CP) and the end product lagging, which leads to a decrease in the content of sans () in the product. When the reaction is carried out at for 163 h, a product with a high content (Cjf) is obtained, even if the particle size of the original carbon-containing material was 20-50 mesh, but in this case the required reaction time This is unacceptably large. In Figure 13, the characteristic peak (CiF) h lies at 10 ° (, 20), and the peak (Cf) at 13.5 "(20 ° C. Fluorine gas pressure is not a determining factor. Generally, the higher the fluorine pressure, the there is no more (c, p) y content in the product, but reactors resistant to very high fluorine pressures and temperatures used do not exist. Generally, nickel or such metals as Monel metal are used as materials for reactors. For this reason, the working pressure range of gaseous fluorine is from 50 mmHg to 1.5 atm, preferably 100760 mm. Hg, which is confirmed by Fig. 14. According to the proposed method, products with different contents are obtained (). However, unlike the known product (cf), the products obtained by the proposed method: are characterized by the absence of non-carbonated carbon and the presence of a new chemical compound - polycarbon monofluoride of the formula (CrP} in an amount of more than 50 mol ...%. The content (С F) in the product cannot be exactly 100%, since the product obtained by the proposed method always contains CP and CPi groups in the supernatant) x particles of the final product. Unlike the product obtained by the proposed methods, the product resulting from the fluorination reaction occurring at a temperature of more than 500 s is characterized by the fact that all peripheral CF groups are thermally decomposed with the formation of gaseous Cp4. The product obtained by the proposed method can theoretically be described by the formula (CF), where x is 0.5-0.75. However, the products actually formed are usually described by the formula (with F, i, where X varies from about 0.58 to 0.82, due to the presence of peripheral CPj and CFj groups. Especially if the quality of the original carbon-containing material is the treatment of petroleum coke, then the value of x increases, since the particles of this material have a very small size and, therefore, the product as a whole has a large surface area occupied by peripheral, CPj and CPj groups. From the component other than (C, P) ", CP2 and CFj groups, the product obtained by the proposed method contains (CP)". The optimum temperature conditions for the preparation of the product of the invention vary somewhat depending on the degree of crystallinity of the original carbon-containing material. when the Franklin P parameter is O or 0.1, the optimum reaction temperature lies within 350-500 ° C. When the Franklin parameter is 0.11-0.45, the temperature optimum lies between 320-450 C. With the parameter Franklin 0.46-0.60 temperature timum reaction is in the range 300-420 C. As indicated VY7 Hsi, the reaction time varies depending on the reaction temperature and the like Typically, for example, when the reaction temperature is of the order, the reaction time may be 50150 hours. When the reaction is carried out at a temperature of about 500 ° C, the reaction time may be 10-100 minutes. In order to obtain a polydicarbon monofluoride of the formula (CiF,), in a directional manner, the reaction temperature is further limited and changed depending on the carbon-containing material used. When the parameter of Franklin P is equal to Yu or about 0.10, then the reaction teletechnology may preferably lie within 350-400s. With a Franklin parameter value of about 0.11-0.45, the reaction temperature may preferably lie in the range of 320-360. With a Franklin P parameter value of about 0.46-0.6, the reaction temperature may preferably lie within 300-3 ° C . When the fluorination reaction of the crushed carbon-containing material is carried out to be straightforward or less, the product yield can reach up to 100% relative not only to the amount of carbon-based material used, but also to the amount of fluorine (as explained in Fig. 15) Such compositions do not contain unreacted carbon. it does not occur at all. According to this, the reaction can be carried out in a closed system or in a batch system. The product obtained as a result of the fluorination of natural graphite at 500 C or less has a low degree of crystallinity and black color, but only when such a product with a low crystallinity is heated in an atmosphere of fluorine, its crystallinity easily increases, and to a varying degree depending on the heat treatment temperature. A determining factor, but as a rule, heat treatment with a duration of 5-10 hours (and up to 120 hours) is usually sufficient to increase the degree of crystallinity of the product to the desired level. The increase in crystallinity depends on the heat treatment temperature. For these purposes, a temperature in the range of temperatures from the fluorination reaction temperature to may be used. Fluorine pressure is not a determining factor, a pressure of at least 50 mm Hg is sufficient. High fluorine pressure is undesirable because high-pressure fluorine gas is dangerous and causes significant equipment corrosion. A maximum pressure of 1.5 atm can be used. Most preferably, the pressure is 760 mmHg. Usually crystallinity can be estimated by the color of the product. As the degree of crystallinity increases, color changes from gray to white. For example, when using natural graphite, the color of the final product changes from gray at 550 ° C to white at 600 ° C. This heat treatment changes only the crystallinity of the product and does not change the F / C ratio. The most preferred degree of crystallinity is determined by the designation of the final product | Ta. For example, a relatively low degree of crystallinity is desirable for products used as cathode material in electroplating. elements of high energy, whereas for lubricants necessary products with high crystallinity. Example 1. 25 mg of Madagascar natural graphite (purity determined by weight of ash, more than 99%) with a particle size of 62-g74 µm is placed in a mold for sample 8 (Fig. 16) and compacted carefully. Gaseous fluorine from the vessel is used. 18 with a purity of 98%. The impurities of the IG in the gaseous fluoride gas are completely removed, the fluorine passes through the drexel 17 cooled to -78 ° C, and the bath 16 filled (the outgoing gas is removed, passes the source gas stream through the bath 15 with soda limestone Natural graphite placed in The sample mold is heated under vacuum (at a pressure of not less than Hg) for about 2 hours to remove traces of moisture contained in graphite. Gaseous fluorine is introduced into the reactor. The reaction is carried out at 375 ° C for 120 h, maintaining the pressure of fluorine at 200 mm Hg. As a result, pores are obtained the black color of the product. Its yield with respect to the amount of used natural graphite is 100%. The fluorine content in the product is determined as follows: The product obtained is burned in a flask with oxygen, and the fluoride released in the form of hydrogen fluoride is absorbed by water. using an electrode with fluorine ions. As a result, an empirical Formula (SGD5) is obtained. The ICA-spectrum of the product is taken on an NZSL — 650-B type spectrophotometer (manufactured by DuPont CO, USA). The spectrum is shown in FIG. 8. From the E5CA spectrum, it can be seen that the fraction of fluorine 0.08 is due to the CF and CF groups formed in the outer regions of the product particles. Thus, it was found that the product is predominantly a compound of the structural formula (CjF). Then the product is heated and the atmosphere of fluorine for 120 hours. The color of the product changes from black to white, but its structure does not change. A radiograph of the product is taken, which is shown in FIG. 2. A device of the type JDX-8 (manufactured by Nikoi Denshi Sha, Japan) is used for this. As a source of x-ray radiation, the Su | IK line is used. obtained by removing the line K with a nickel filter. The measurement conditions are as follows;
Voltage in the tube and current 35 kV, 10 mA
Scanning speed of the goniometer 1 / min Target -1 -1-0.10 N
Recording Device Constant
time 1 sec, paper moving speed 1 cm / min
Example 2. The same sequence of operations as in Example 1 is repeated, except that the reaction is carried out under a fluorine pressure of 760 mm Hg. at 20 hours. The result is a black product (C Fojg) which is heat treated at 600 ° C in an atmosphere of fluorine (200 mm Hg) for 6 hours. The color of the product varies from black to white, but the structure the product itself does not change.
Example 3. The procedure described in example 1 is repeated. The temperature is 450 ° C and the reaction time is 10 hours. For DSShne heat treatment of the product obtained in example 1, in the atmosphere of fluorine (200 mm Hg) for 1 9 The empirical formula changes and becomes (CF). The product formed (cP (7) t) is more recently heated under a fluorine atmosphere (200 mm Hg) for 120 hours, but the F / C ratio does not change. This indicates that the product of the empirical formula () c contains unreacted graphite, which is also confirmed by microscopic studies. X-ray and E5CA spectra show that the product of the formula (CFqjj is a compound (
Examples 4 and. 5. Repeat the same procedure as in Example 1, except that instead of natural graphite, heat-treated petroleum coke is used as the starting material (Franklin parameter, 31, heat treatment: 2800 ° C for 30 minutes) with a particle size of more than 400 mesh (less than 37 MKN. Tag-sheratura reaction in example 4, in example 5, the reaction time is 5 and 100 hours, respectively.
Products of the formula lCFo.7) n and (CP (| oO are heat treated under an atmosphere of fluorine (200 mm Hg) for 120 h without changing their structure. The color of the products changes from black to white.
Example b. The same procedure as in example 1 is repeated, except that instead of natural graphite, petroleum coke is heat treated (Franklin parameter R 0.6, heat treatment for 30 min) with a particle size more than 400 mesh (less than 37 microns). The reaction temperature, time 90 hours
The product of the formula (with Rci) is heated in an atmosphere of fluorine (200 mm Hg) at 550 ° C for 120 h without changing its structure. The color of the product varies from black to white.
The polydicarbonmonofluoride obtained has a crystalline structure, and the distance between the intermediate layers is approximately 9.0 A. The length of the C – T bond and the C – C bond in (,) n is about 1.35 Au and 1.54 A, respectively.
Compound (C2), has the following properties and characteristics.
The immersion heat for a black sample is 55 erg / cm2, for a white one 53 erg / cm i. The heat of immersion (Cf) obtained as a result of the reaction at BOO-C for 120 h in the atmosphere of fluorine (200 mm Hg 36 erg / cm. From the above results it follows that (C, Characterized by high social activity, wetting, resistance to dyes, water repellency properties, etc. Wetting resistance () “is lower compared to, (C) but it can give better results if CCjf) is used as a cathode material in high-energy galvanic cells.
From the DTA curves it can be seen that the temperature of thermal decomposition (CjF obtained as a result of reaction at 375 ° C for 120 hours and having a low crystallinity in an argon atmosphere is. When cooked for 120 hours, the crystallinity of the compound (C1p) becomes maximum , and the temperature of thermal decomposition in an argon atmosphere is already 570 ° C. The thermal decomposition temperature (CG) "obtained by fluorinating the same natural graphite at 600 ° C for 120 hours at a fluorine pressure of 200 mm Hg is 605 ° C (CP) get ny under such conditions has a maximum crystallinity.
Co-resistance () “(black and white samples), 10 ohm / cm. Specific resistance (, CF) n S Ohm / cm
Specific surface (nitrogen adsorption method), Black (CjF) ,, 28 white (СР) „117. white (CP) "122.
In the IR spectra of the black sample, absorption due to the C – P bond oscillation occurs at 1221 cm, for a white sample (CjF) obtained by warming the specified black sample (; C, P), for 120 h in the atmosphere ({Lagoram (200 km Hg), absorption following the valence vibration of the C -F link is observed at the same wavenumber, namely 1221. Characteristic, realistic 1st band of the bond diagram of the C-x white bond
tsa | CF) lies at cm. It is quite occated (but that (C2) n | SG) have a different structure.
The chemical compound () is formed at a temperature of 300-500 ° C. The color of the product thus obtained is black, but during thermal processing it will outgrowth to gray (measured, at), and then to white (approximately at ..
Table 1
The relationship between the size of the formulas) (natural graphite:
Comparative example. particles and the ratio F / C products / (empirical fluorine, 200 mm Hg) T a b l and c a 2.
Ten / tofair oSpaSomKa npu-SffO C
.
 The confluence fiOv 0, Sg in atmospheres fluorine
(black) (SfAMU)
3SO CHUfOO6t№
Temperature with
(001)
go
GO fut, l.
(wo)
fo
ff
gbp
K.J
 (Cif) n
OYOPYAUTCHMY (Cf) n
/
9.9 9 .9
h X.
g
6.0
five;
3.9
H
1.0
3fa 0fffffofoo
TfMfffpamypaiC
LS) K-P9nt conquer
ten
If
(90f) FIG.
(100)

fO
ze (f
ui.S
i9f gzo iSf Cij Energy / t s9 zi, EU
19S-29028jrpg
Cis sve, tV fuz.S
ClfSbC-f
C to g of C-C (impurities)
Z80 .7
cent C-F
Ct sA C-CfCzf (.stezhgggItrich.)
01Я31 С-С
(bring)
3000 2000
.ro
YuOOSh650
Into the number. fH-
4000 3000 mo
woo700650
SonHOtoe number, w-i capribo, 120h Obtained at J75V, 600. С Temperature, Сlput.t2 Obtained at 500C, 120h Heat of odoaffom 120V
5 10 15 20 20-50 nets 200-250shn UNIf 20-50 MKU 200-250mesh 20-50les 200-250mesh 00 neil
5W
too n pm: f, m. 200fifi.pni.cm.
150 fOOnfi fm.cm

x
 ndnn.pm ...- 4j
s

-A
 yp
 fOOftfi.pm cm 5:
- tuvnn.fiii I;
;
Y ZOOfiMpm.cm Yuopm pm.cm
f
50
. . cm. 200 MH fm. cm
350,100 ftM. ptn.cm
5 W / 5 20 2c {) FIG. 14
500
SOO Temperature, V of FIG. /five
HX
13

fui.lS
9
eleven

权利要求:
Claims (1)
[1]
1. A METHOD FOR PRODUCING POLYFLUOROCHLORIDE, comprising treating a carbon-containing material with fluorine gas at 300-500 ° C, characterized in that, in order to increase the yield of polyfluorocarbon of formula (C ₇ F) _n and to simplify the process of and - g with the aim of ® it was processed by atmogase-like fluorine for one hour at a pressure of at least Hg
in
SP □ About

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同族专利:

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公开号 | 公开日

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DE2736861C3|1982-04-22|

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DE2736861B2|1981-07-02|

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JPS612609B2|1986-01-27|

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NL175900C|1985-01-16|

---

IT1084178B|1985-05-25|

---

CH640198A5|1983-12-30|

---

NL7709216A|1978-08-24|

---

DE2736861A1|1978-08-24|

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FR2384715B1|1982-04-23|

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NL175900B|1984-08-16|

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GB1585878A|1981-03-11|

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FR2384715A1|1978-10-20|

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JPS53102893A|1978-09-07|

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US4139474A|1979-02-13|

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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JP52017823A|JPS612609B2|1977-02-22|1977-02-22|

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