US2967808A - Inhibition of decomposition of amalgam - Google Patents
Inhibition of decomposition of amalgam Download PDFInfo
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- US2967808A US2967808A US755073A US75507358A US2967808A US 2967808 A US2967808 A US 2967808A US 755073 A US755073 A US 755073A US 75507358 A US75507358 A US 75507358A US 2967808 A US2967808 A US 2967808A
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- brine
- amalgam
- decomposition
- percent
- alkali metal
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- 229910000497 Amalgam Inorganic materials 0.000 title claims 2
- 238000000354 decomposition reaction Methods 0.000 title 1
- 230000005764 inhibitory process Effects 0.000 title 1
- 150000002334 glycols Chemical class 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims 1
- 150000001298 alcohols Chemical class 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 claims 1
- 239000012267 brine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 claims 1
- 150000002170 ethers Chemical class 0.000 claims 1
- 150000002440 hydroxy compounds Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 229920001515 polyalkylene glycol Polymers 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
- C25B1/36—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in mercury cathode cells
Definitions
- the invention relates to inhibiting the decomposition of an amalgam. More particularly, it relates to inhibiting the decomposition and/or reaction of an alkali metal amalgam during the production thereof in the electrolyzer chamber of a chlorine cell which employs a mercury cathode in the electrolysis of an alkali metal chloride electrolyte. Reactivity of the alkali metal amalgam during electrolysis, although appearing to consist of both decomposition and complex reactions with the aqueous electrolyte, will be referred to hereinafter merely as the decomposition thereof for simplicity of expression.
- a conventional cell and method of producing chlorine is to electrolyze an alkali metal chloride brine, e.g., an aqueous solution of NaCl, to yield chlorine gas at the anode and the alkali metal as an amalgam on a mercury cathode, ⁇ the amalgam being subsequently decomposed in the presence of water in a separate chamber or chambers to yield the alkali metal hydroxide and hydrogen as end products and mercury for re-use in the electrolysis.
- metal hydroxide and chlorine employing such cell and method there has heretofore been a loss in ef'liciency, an appreciable part of which is due to the decomposition admixed with the alkali metal chloride brine employed f in such cells.
- the compounds which can be employed in the practice of the invention as additives to such brine y electrolytes are the alkylene glycols, monoand poly alkylene glycol monoethers, halo-substituted derivatives of such glycols and ethers, epihalohydrins, and higher morV lecular weight saturated alcohols having at least 5 car Y bon atoms.
- Examples of such hydroxy compounds are dipropylene glycol, epichlorohydrin, cyclohexanol, 2 methoxyethanol, 2(2-ethoxyethoxy)ethanol, ethylene glycol, Z-ethoxyethanol and ethylene chlorohydrin.
- Thehydroxyl group is thought to be an essential substituent of the inhibitor employed according to the invention.
- Epihalohydrins are considered to be within the class because they assume characteristics of such hydroxy compounds as the glycols and their ethers, apparently due to hydrolysis at the oxygen bridge.
- Lower molecular weight alcohols cannot be employed because of their tendency to react in a similar manner to, although less violent than, water with an alkali metal amalgam.
- Hydroxyl-containing compounds having acidic properties e.g., carboxylic acids, phenol, cresols, and the like, cannot be used.
- the alcohol should contain at least tive carbon atoms to be sufficiently unreactive with the amalgam.
- the additives which include both liquids and solids usually exist under normal conditions as liquids f and may be advantageously stirred into the electrolyte In the electrolytic production of an alkali of the alkali metal amalgam during the electrolysis.
- the invention is an improved electrolyte for and method of producing chlorine and an alkali metal amalgam by the electrolysis of an alkali metal chloride brine wherein a water-soluble organic hydroxy compound is either prior to the electrolysis or intermittently or continuously during the electrolytic process to achieve the desired effect of their use in accordance with the invention.
- Each of the additives is a Well-known, readily accessible, and relatively inexpensive material.
- the amount of additive to employ is not sharply critical and may be calculated either as a percent by volume or percent by weight based on the volume or 4weight of brine. For'convenience, the percent by volume is usually used since the specific gravity of the additive is not greatly ⁇ d iierent from that of the brine.
- the amount employed in the practice of the invention is small.
- At least 0.001 percent byvolume should be employed. It is recom-n mended that between 0.005 and 0.03 percent by volumek be employed. Greater amounts, e.g., .05 percent or more maybe employed but are considered uneconor'nical. 0.02 percent appears to be about the optimum amount to add, based on the volume of the alkali metal chloride' brine.
- Sodium amalgam feed tube 14 provided with funnel 16 leading into dish 12 and vertically positioned graduated cylinder 18 having dome-shaped base 20 resting on the bottom of jar 1), which forms a gas-collecting means about dish 1-2, 5 and having petcock assemblyl 22 and nipple 24 in -the upper part thereof for the attachment of an exhaust means.
- Sodium amalgam 26A is shown onv the floor of dish 12. In dish 12 and partially submerged in amalgam 26 is graphite anode 28 consisting of two verticallypositioned 1/4 plates separated by an insulator.
- Sodium chloride brine 30 is shown in Pyrex jar and in tube 14 at the Vsame level as 15 in jar 10, and in tube 14 at the same level as in jar 10, and in cylinder 18 extending to the top thereof, ⁇ tlie brine gam in an alkali metal chloride bath by the presence of an inhibitor in accordance with the invention was then shown in the examples below .by following the procedure and employing the apparatus and the same concentration of sodium chloride brine as in the conditioning steps above except that in each of the examples, an increasing amount of an inhibitor was addedto the brine, according to the invention, contained in jar 10 as shown in Figure l.
- the amounts of the inhibitor were increased up to 0.02 percent by volume based upon the volume of sodium chloride brine.
- the effect on decomposition efiiciency is set out in table form in Table I for additions of 0.0l and 0.02 percent by volume of inhibitor and graphically in Figure 2 for the additions shown, up to 0.02 percent.
- the graphite cathode was iirst conditioned by repeat- 55 ing the following series of conditioning steps several times until the volume of hydrogen gas evolved per minute was stabilized, i.e., was substantially uniform:
- Graphite cathode 28 was placed in position in dish 12.
- the rate of hydrogen gas collecting in the graduated upper portion of cylinder 18 per minute'became stabilized at an average of 0.34 milliliter per minute.
- the decomposition eciency continually lessened withincreased amounts of the inhibitor up to 0.02 percent by volume, except for cyclohexanol which was somewhat more eiective than the other inhibitors in small amounts (on the order of 0.001 percent) but which leveled oi with a slightly lessening inhibiting eiect at about 0.015 percent.
- OH radical in the organic group appears essential to the practice of the invention. Furthermore, the presence of two OH radicals such as in the case of the dipropylene glycol, appears to enhance the benecial eiect upon the suppression of the decomposition of the sodium amalgam.
- the effective inhibition of the decomposition of an alkali metal amalgam has direct application when the inhibitor is added to a mercury cathode type chlorine cell employing an alkali metal chloride electrolyte.
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Description
Jan. 10, 1961 R. s. KARPIUK 2,967,808
INHIBITION oF DEcoMPosITIoN oF AMALGAM Filed Aug. 14, 1958 I/o/ume Percen//n/u'//or INVENTOR. Roef/ .5. /fofol'u TTORNEY INHIBITION F DECOMPOSITION OF AMALGAM Robert S. Karpiuk, Midland, Mich., assignor to The Dow `Chemical Company, Midland, Mich., a corporation of Delaware Filed Aug. 14, 1958, Ser. No. 755,073
3 Claims. (Cl. 204-99) The invention relates to inhibiting the decomposition of an amalgam. More particularly, it relates to inhibiting the decomposition and/or reaction of an alkali metal amalgam during the production thereof in the electrolyzer chamber of a chlorine cell which employs a mercury cathode in the electrolysis of an alkali metal chloride electrolyte. Reactivity of the alkali metal amalgam during electrolysis, although appearing to consist of both decomposition and complex reactions with the aqueous electrolyte, will be referred to hereinafter merely as the decomposition thereof for simplicity of expression.
A conventional cell and method of producing chlorine is to electrolyze an alkali metal chloride brine, e.g., an aqueous solution of NaCl, to yield chlorine gas at the anode and the alkali metal as an amalgam on a mercury cathode, `the amalgam being subsequently decomposed in the presence of water in a separate chamber or chambers to yield the alkali metal hydroxide and hydrogen as end products and mercury for re-use in the electrolysis. metal hydroxide and chlorine employing such cell and method, there has heretofore been a loss in ef'liciency, an appreciable part of which is due to the decomposition admixed with the alkali metal chloride brine employed f in such cells. The compounds which can be employed in the practice of the invention as additives to such brine y electrolytes are the alkylene glycols, monoand poly alkylene glycol monoethers, halo-substituted derivatives of such glycols and ethers, epihalohydrins, and higher morV lecular weight saturated alcohols having at least 5 car Y bon atoms. Examples of such hydroxy compounds are dipropylene glycol, epichlorohydrin, cyclohexanol, 2 methoxyethanol, 2(2-ethoxyethoxy)ethanol, ethylene glycol, Z-ethoxyethanol and ethylene chlorohydrin. Thehydroxyl group is thought to be an essential substituent of the inhibitor employed according to the invention. Epihalohydrins are considered to be within the class because they assume characteristics of such hydroxy compounds as the glycols and their ethers, apparently due to hydrolysis at the oxygen bridge. Lower molecular weight alcohols, however, cannot be employed because of their tendency to react in a similar manner to, although less violent than, water with an alkali metal amalgam. Hydroxyl-containing compounds having acidic properties, e.g., carboxylic acids, phenol, cresols, and the like, cannot be used. The alcohol should contain at least tive carbon atoms to be sufficiently unreactive with the amalgam. The additives, which include both liquids and solids usually exist under normal conditions as liquids f and may be advantageously stirred into the electrolyte In the electrolytic production of an alkali of the alkali metal amalgam during the electrolysis. A, mercury cell, of the type described in U.S. Patent.
Attempts have been made to improve the efficiency ofY mercury cathode-type chlorine cells by the addition of inorganic stannates, borates, silicates, or pyrophosphates to the electrolyte. These attempts have not been suili-` ciently successful in the inhibition of the decomposition of the alkali metal amalgam to justify their being adopted generally in the production of chlorine employing such cells.
There exists, therefore, a desideratum in the art of chlorine production by the electrolysis of an alkali metal chloride brine, wherein the alkali metal is recovered as an amalgam on a mercury cathode, for an improved electrolyte and method employing such electrolyte which is substantially more eilicient due to the inhibition of the decomposition of the alkali metal amalgam during the electrolysis of the brine.
It is an object of the invention to provide such an improved electrolyte and a method of use thereof wherein the decomposition of the amalgam being formed is suppressed or inhibited thereby improving the efficiency of the electrolytic production of mercury cathode type cells.
The method and means by which this and related objects of the invention are attained is made clear in the ensuing description and are particularly defined in the appended claims.
The invention is an improved electrolyte for and method of producing chlorine and an alkali metal amalgam by the electrolysis of an alkali metal chloride brine wherein a water-soluble organic hydroxy compound is either prior to the electrolysis or intermittently or continuously during the electrolytic process to achieve the desired effect of their use in accordance with the invention. Each of the additives is a Well-known, readily accessible, and relatively inexpensive material. The amount of additive to employ is not sharply critical and may be calculated either as a percent by volume or percent by weight based on the volume or 4weight of brine. For'convenience, the percent by volume is usually used since the specific gravity of the additive is not greatly` d iierent from that of the brine. The amount employed in the practice of the invention is small. At least 0.001 percent byvolume should be employed. It is recom-n mended that between 0.005 and 0.03 percent by volumek be employed. Greater amounts, e.g., .05 percent or more maybe employed but are considered uneconor'nical. 0.02 percent appears to be about the optimum amount to add, based on the volume of the alkali metal chloride' brine. An apparatus of the type schematically shown in',l Figure l was employed to demonstrate the elfects of the- Water-soluble organic hydroxy compounds on the decom-l position rate of a sodium amalgam when added to alf alkali metal chloride brine in a primary cell in which an alkali metal amalgam and pieces of graphite serve as the anode and cathode, respectively, of the cell. De-' composition efiiciency is a measure of the decompositiony of the alkali metal amalgam in the testing apparatus' used. It is percent, as shown in Figure 2, when no inhibitor is present. Decomposition eieiency is defined Volume of H2 evolved per second from inhibited brine X100? Volume of H2 evolved per second from o substantially pure brine The rate of decomposition of a prepared sodium amalgamv in a speciic concentration of sodium chloride brine was ascertained by determining the volume of hydrogen` evolved during a measured period of time employing the apparatus shown in Figure 1. The decomposition el`` ciency of the sodium amalgam in the NaCl brine accord-, ing to the invention as thus determined is set outin The apparatus "f 'Figure 1` comprises Pyrex jar 1o.
Patented Jan. 1o, 1961.,
TABLE I Eeci` on decomposition of amalgam in brine by presence of inhibitors Properties oi Decomposition Inhibitors Eicency Example Inhibitor Added to Formula of Inhibitor Percent the Brine Inhibitor Mol. Density by Volume Wt. at C.
1 Dipropylene glycol (CHsCEOH-CHQMO 134. 17 1. 022 51 48 2 Epichlorohydrn CHz-CH--CHg-Cl 92. 53 1. 801 64 58 Cyclohexanol CsHnOH 100.16 0. 9499 63 63 2methoxycthanol CHa- O-CHz-CHz- OH- 76.09 0. 966 75 64 2-(2-ethoxyethoxy) ethanol 01H5-OCH2-CH;-OCH2CH7-O 134. 17 0. 9902 76 68 Ethylene glycol HO-CHz-CHz-OH 62. 7 1.1155 76 76 2ethoxyethanol CzH5OCH2-CH2-OH 90.12 0. 9311 88 76 Ethylene chlorohydrm Cl- CHTCHTOH 80. 52 1. 213 93 88 no inhibitor Nnna 100 100 being drawn up into 18 by exhausting the air therefrom as explained hereinafter. 4
The practice of the invention will be illustrated by examples showing the rate of decomposition of an amalgam in a sodium chloride brine containingan inhibitor according to the invention in contrast to the rate of decomposition of the sodium chloride brine to which no 60 inhibitor is added.
To illustrate the practice of the invention, the following procedure was-followed employing an apparatus of the type shown in Figure 1: Y
The graphite cathode was iirst conditioned by repeat- 55 ing the following series of conditioning steps several times until the volume of hydrogen gas evolved per minute was stabilized, i.e., was substantially uniform:
A brine consisting of 300 grams of chemically pure sodium chloride dissolved in enough water to make tive liters was placed in jar 10. Petcock 22 was opened and vacuum applied at nipple 24 thereby exhausting cylinder 18 of ail and causing the brine to rise in cylinder 18, as shown, until it reached petcock 22 at which time petcock 65 22 was closed and the vacuum discontinued. The temperature of the brine was 25 C.
250 grams of sodium amalgam. consisting of 0.28 percent by weight of sodium, the balance being mercury, were then poured into funnel 16 and down tube 14, col- 70 lecting at the bottom of dish 12 as shown.
The rate of hydrogen gas collecting in the graduated upper portion of cylinder 18 per minute'became stabilized at an average of 0.34 milliliter per minute.
The effect on decompositionof an alkali metal amal- A study of Table I and Figure 2 shows the decomposi- 5 tion eiciency of the sodium amalgam uninhibited brine to` be percent and that additions of various inhibitors to the pure brine containing the amalgam in accordance with the invention substantially lowered this efiiciency by inhibiting the decomposition thereof. Figure 2 also shows that when as little inhibitor was added as 0.001 percent by volume based on the volume of NaCl brine, the inhibiting effect on the decomposition of the amalgam was readily apparent and that this effect became. more marked, i.e., the decomposition eciency continually lessened withincreased amounts of the inhibitor up to 0.02 percent by volume, except for cyclohexanol which was somewhat more eiective than the other inhibitors in small amounts (on the order of 0.001 percent) but which leveled oi with a slightly lessening inhibiting eiect at about 0.015 percent. A further` study of Figure 2 shows that an amount of an inhibitor of at least 0.01 percent by volume should be added, that 0.02 percent appears to be an optimum amount to add, andthat in general some increased inhibiting effect continuesbeyond an` amount of 0.02 percent but by extrapolation of the curves such increased eiectappears inconsequential beyond say 0.03 percent, and clearly uneconornical beyond about 0.05 percent by volume of the alkali metal chloride bath.
Further examination of the table and Figure 2 shows the relative diminution of decomposition of the amalgam when the different inhibitors are used in accordance with the invention. For example, when 0.02 part by volurne of dipropylene glycol, based upon the volume of the brine, is added thereto, the decomposition is reduced by 52 percent. The least eifective of the additives of the asezsos invention employed was ethylenechlorohydrin which showed a diminution of the decomposition of the sodium amalgam by 12 percent.
The presence of the OH radical in the organic group appears essential to the practice of the invention. Furthermore, the presence of two OH radicals such as in the case of the dipropylene glycol, appears to enhance the benecial eiect upon the suppression of the decomposition of the sodium amalgam.
The effective inhibition of the decomposition of an alkali metal amalgam, as demonstrated by the example, has direct application when the inhibitor is added to a mercury cathode type chlorine cell employing an alkali metal chloride electrolyte.
To illustrate the invention, 0.02 volume percent of dipropylene glycol based on the volume of the NaCl brine was added thereto in the electrolyzer chamber of a cell in a commercial chlorine-producing unit. The eiciency of the cell rose 7 percent over its production eiciency prior to such addition. After 3 days the production eiiciency decreased to its earlier eciency. 0.02 volume percent of dipropylene glycol was again added to the cell upon which the production eiciency again rose by 7 percent.
The examples above show that the presence in the brine used in a mercury cathode type cell of a water-soluble organic hydroxy compound illustrated by alkylene glycols, monoand polyalkylene glycol monoethers, halosubstituted glycols and ethers and such hydroxy-forming compounds as epichlorohydrin, and high molecular Weight saturated alcohols, suppress or inhibit the decomposition and/ or reaction of the alkali amalgam formed at the cathode. Such decomposition during electrolysis, when uninhibited, decreases the efficiency of the cell to a point where it seriously aiects the output. Markedly raising the eiciency of such cells by the addition of a readily available, safe, low-cost inhibitor has an extensive economic impact upon chlorine and alkali hydroxide production.
Having described the invention, what is claimed and desired to be protected by Letters Patent is:
1. The method of producming chlorine by electrolysis of an alkali metal chloride brine employing a mercury cathode consisting of admixing with the brine between 0.001 and 0.05 percent by volume of a water-soluble organic hydroxy compound unreactive with alkali metal amalgams selected from the class consisting of alkylene glycols, monoand polyalkylene glycol monoethers, halosubstituted derivatives of said glycols and ethers, epihalohydrin, and higher molecular Weight saturated alcohols containing at least 5 carbon atoms.
2. The method according to claim 1, wherein the organic hydroxy compound is dipropylene glycol.
3. The method according to claim 2, wherein the dipropylene glycol is admixed in an amount between 0.01 and 0.03 percent by volume based upon the volume of brine.
References Cited in the iile of this patent UNITED STATES PATENTS 1,868,710 McCullough July 26, 1932 2,668,225 Livingstone Feb. 2., 1954 FOREIGN PATENTS 465,365 Canada May 23, 1950
Claims (1)
1. THE METHOD OF PRODUCING CHLORINE BY ELECTROLYSIS OF AN ALKALI METAL CHLORIDE BRINE EMPOLYING A MERCURY CATHODE CONSISTING OF ADMIXING WITH THE BRINE BETWEEN 0.001 AND 0.05 PERCENT BY VOLUME OF A WATER-SOLUBLE ORGANIC HYDROXY COMPOUND UNREACTIVE WITH ALKALI METAL AMALGAMS SELECTED FROM THE CLASS CONSISTING OF ALKYLENE GLYCOLS, MONO- AND POLYALKYLENE GLYCOL MONOETHERS, HALOSUBSTITUTED DERIVATIVES OF SAID GLYCOLS AND ETHERS, EPIHALOHYDRIN, AND HIGHER MOLECULAR WEIGHT SATURATED ALCOHOLS CONTAINING AT LEAST 5 CARBON ATOMS.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US755073A US2967808A (en) | 1958-08-14 | 1958-08-14 | Inhibition of decomposition of amalgam |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US755073A US2967808A (en) | 1958-08-14 | 1958-08-14 | Inhibition of decomposition of amalgam |
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| Publication Number | Publication Date |
|---|---|
| US2967808A true US2967808A (en) | 1961-01-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| US755073A Expired - Lifetime US2967808A (en) | 1958-08-14 | 1958-08-14 | Inhibition of decomposition of amalgam |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1868710A (en) * | 1929-08-02 | 1932-07-26 | Lee W Mccullough | Current controlling or regulating device |
| CA465365A (en) * | 1950-05-23 | Imperial Chemical Industries Limited | Electrolysis of aqueous solutions | |
| US2668225A (en) * | 1951-03-20 | 1954-02-02 | Livingstone Engineering Compan | Vaporizable liquid electrode boiler |
-
1958
- 1958-08-14 US US755073A patent/US2967808A/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA465365A (en) * | 1950-05-23 | Imperial Chemical Industries Limited | Electrolysis of aqueous solutions | |
| US1868710A (en) * | 1929-08-02 | 1932-07-26 | Lee W Mccullough | Current controlling or regulating device |
| US2668225A (en) * | 1951-03-20 | 1954-02-02 | Livingstone Engineering Compan | Vaporizable liquid electrode boiler |
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