序号 专利名 申请号 申请日 公开(公告)号 公开(公告)日 发明人
141 Improvements in or relating to the preparation of glycerine GB1117655 1955-04-18 GB768779A 1957-02-20
Glycerin is prepared by hydrolysing a 1-halo-2.3-epoxy-propane by contacting it with an aqueous solution of an inorganic carbonate at a temperature between 130 DEG and 200 DEG C. for a period between about 5 and 20 minutes in the presence of carbon dioxide under a pressure sufficient to maintain the reactants in the liquid phase. The "inorganic carbonates" are inorganic carbonate or bicarbonate salts or mixtures thereof. The preferred inorganic carbonates are the alkali metal carbonates and bicarbonates. The process may be carried out batchwise, intermittently or continuously. The starting 1-halo-2.3-epoxypropane can be formed in the reaction mixture from the corresponding dihalohydroxypropane by using an increased amount of sodium carbonate. In the examples: (a) 1-chloro-2.3-epoxy propane, produced by steam stripping an allyl chloride chlorohydrination product in the presence of a base, is hydrolysed by contacting with sodium carbonate under varying conditions to give glycerin. Specification 711,657 is referred to.
142 Process for preparing glycerol FR1129976D 1955-04-18 FR1129976A 1957-01-29
143 A process for recovering glycerine DEJ0006609 1952-11-25 DE940522C 1956-03-22 BLAIR JAMES; MCLELLAN THOMAS AUCOTT
144 Improvements relating to the refining of glycerine GB2105948 1948-08-10 GB650438A 1951-02-21
Glycerine which has been obtained by the transesterification of fatty material having an acid value of at least 1 by a low molecular weight alcohol first under alkaline and then under acid conditions, is purified by neutralizing the acidic glycerine with an oxide or hydroxide of an alkaline earth metal followed by heating with an ammonium halide and removal of insoluble material. The acidic glycerine may be neutralized either before or after separation from the acidic esterification mass. The halide-treated glycerine may be extracted with methanol, ethanol, propanol, or butanol, or with acetone, or it may be dissolved in one of these alcohols and acetone added until a precipitate just begins to form, heated, insoluble matter removed, and the solvent distilled off. The glycerine may finally be distilled under reduced pressure or co-distilled with a mineral oil of similar boiling point. The process is normally conducted under relatively water-free conditions, an oxide such as barium oxide being therefore preferable to an hydroxide as a neutralizing agent. If very acid starting materials have to be dealt with, which would give rise to the presence of considerable amounts of water, the transesterification reaction is carried out so that water of reaction is continuously removed by refluxing or mechanical separation. According to examples, peanut and hydrogenated fish oils are treated with methanol in presence first of caustic soda and then of sulphuric acid, barium oxide or calcium hydroxide added, and the mixture then heated with ammonium chloride with or without methanol to reduce the viscosity. The alcohol is removed by distillation and the glycerine filtered and vacuum distilled. Specifications 579,767 and 647,174 are referred to.
145 FR962037A - FR962037D FR962037A 1950-05-27
146 Improvements in or relating to process of purifying glycerine containing ionizable impurities GB2204246 1946-07-24 GB633343A 1949-12-12
Crude glycerine solutions containing at least 1000 parts per million of ionisable impurities are purified by passing them through a number of pairs of ion exchangers, the first member of each pair being a cation-active or hydrogen zeolite exchanger and the second an anion exchanger. The process is continued while the influent to the final anion exchanger contains less than about 600 parts per million of anions and 50 parts per million of cations, or while the pH of the influent to the final anion exchanger is at least 3 and/or that of the effluent from such exchanger is at least 4. It is stated that the use of more than four pairs of ion exchangers is not economical. The purified glycerine may be finally distilled in a relatively simple still and a product of high quality obtained. The process is preferably employed with relatively dilute solutions such as 5 to 20 per cent glycerine, but may also be used with glycerine containing only 1 or 2 per cent of water. In such cases the final distillation step may be eliminated. The anion and cation active materials are regenerated after use in the conventional manner by treatment with dilute solutions of alkali or acid solutions respectively and subsequent washing with water. As cation-active materials may be used a resinous material prepared by reacting furfurylacetone sulphonate with furfural (see U.S.A. Specification 2,372,233), aldehyde condensation products of a -furyl substituted organic sulphonates (see U.S.A. Specification 2,373,152), polyhydric phenolaldehyde condensation products such as catechol-tannin-formaldehyde, aromatic sulphonic acid-formaldehyde condensation products (see U.S.A. Specification 2,204,539), or the carbonaceous zeolites, i.e. sulphated or sulphonated carbonaceous materials such as coal, peat, or lignite. As anion-active materials may be used resins prepared from guanidine, guanyl urea, and biguanide as prepared according to Specification 561,896, [Group IV], or the aldehyde condensation products of m-phenylene diamine, biguanide, guanyl urea, substituted guanidines such as methyl guanidine, substituted biguanidines such as phenyl biguanide, polyethylene polyamines, &c.
147 Continuous production of crude glycerin GB2273646 1946-07-30 GB617930A 1949-02-14
A method of processing glyceride fats to produce fatty acids and glycerin comprises subjecting preheated water and preheated fat to continuous high temperature, high pressure hydrolysis and continuously subjecting the sweet water issuing at high temperature and high pressure from the hydrolysis to multiple stage vaporization without the application of extraneous heat to produce crude glycerin in concentrated form, this multiple stage treatment including an initial expansion stage to a super-atmospheric pressure below that at which the countercurrent hydrolysis is performed, a final expansion stage to a subatmospheric pressure, and at least one intermediate expansion stage to an intermediate pressure, part of the heat contained in p the vapours from each stage except the last being employed to heat the liquid in the succeeding stage. The fatty material entrained in the resulting crude glycerine may be separated out by gravity settling, centrifuging, or other convenient means, whereby crude glycerine suitable for distillation is produced. Apparatus is described in which the glycerin is concentrated from sweet water to crude in four successive expansion stages. Specification 617,929 and U.S.A. Specification 2,156,863 are referred to.
148 Glycerol substitutes DEZ0025649 1940-01-27 DE744528C 1944-01-20 SCHULZE DR PHIL WERNER
149 Method and apparatus for extracting glycerine residue of roasters FR859932D 1939-06-07 FR859932A 1941-01-02
150 Process for extracting the glycerol from the liquid containing FR855839D 1938-05-17 FR855839A 1940-05-21
151 Improvements in or relating to the treatment of liquid distillery residues GB2173138 1938-07-21 GB518611A 1940-03-04
518,611. Alkali metal compounds ; glycerine. BAUDOT, J. July 21, 1938, No. 21731. Convention date, July 21, 1937. [Classes 1 (ii) and 91] Vinasse is concentrated and treated with sulphuric or other acid to coagulate gums and colloids, which are filtered off. The filtrate is further concentrated until potassium salts crystallize, and is again filtered. Lime is added to the liquid to precipitate calcium salts, which are filtered off, and glycerine is extracted from the residual liquid by distillation, extraction with a solvent &c. The solid products from the several stages may be mixed together and used as fertilizer. In a modification, lime is added immediately after the first filtration, and the mixture is further concentrated and filtered.
152 Improvements in process and apparatus of producing an anhydrous soap and glycerine GB2813537 1937-10-15 GB504118A 1939-04-17
504,118. Making soap; soap powders. DEHN, F. B. (Lorenz Patents Corporation) Oct. 15, 1937, No. 28135. [Class 91] Soap and glycerine are continuously produced by spraying a fat or oil and alkali into a stream of superheated steam maintained above the melting point of anhydrous, soap, the reaction being effected in a retort at subatmospheric pressure, whereupon the volatile products and soap are removed. An apparatus consists of two chambers 1, 2 connected through a rotary fluid-tight feed hopper 19. The chambers 1, 2 are provided with jackets 9, 12, 16, through which heated mineral oil passes. The raw materials are fed in calculated amounts to the chamber 1 at about 150 to 300‹ C:, through pipes 34 (fat) 35 (alkali), 36 (fillers), 37 (superheated steam), which communicate with annular manifolds provided with jets 38 ... 41. The jets are inclined from a radial position whereby a thorough mixing and a swirling motion is imparted to the sprayed materials. Volatile products pass through a perforated diaphragm 27 to a vacuum condenser through a pipe 26. The rotary hopper 19 is provided with pockets 24, whereby the soap particles are fed on to a rotor 50 provided with curved deflector plates mounted at the top of the chamber 2, which is filled with inert gas such as nitrogen, carbon dioxide or steam at a temperature below the melting point of the soap. The soap is thereby separated into particles which harden as they fall to the bottom of the chamber. They are then removed by a screw conveyer 53. If desired a solid hydrated soap is made by admitting a measured amount of water and fillers through the pipe 60, whereupon the anhydrous soap particles and water are mixed by an agitator 51, and the resulting molten soap is drawn off through a pipe 64. Specification 504,117 is referred to.
153 Improvements in process of producing an anhydrous soap and glycerine GB2813437 1937-10-15 GB504117A 1939-04-17
504,117. Making soap ; soap powders DEHN, F. B. (Lorenz Patents Corporation) Oct. 15, 1937, No. 28134. [Class 91] Soap, in anhydrous form, and glycerine are continuously produced by spraying fat, oil, or wax, and caustic alkali solution into a reaction chamber, and passing the co-mingled sprays into a stream of superheated steam continuously flowing through the chamber whereby immediate saponification is effected, whereupon the anhydrous soap 'and glycerine are separated from the water and unsaponifiable constituents. Cottonseed oil from a tank A and caustic alkali from a tank B are pumped, in equivalent amounts, into a heater D to which steam at 250-300‹ C. is admitted from a superheater C, and passes therethrough to the exit pipe 7 ; steam is also fed into a chamber E through a pipe 3. The intimately mingled alkali and oil pass through a spray jet 24, and saponification is rapidly effected. Anhydrous soap as a dry powder falls to the floor while steam, glycerine vapours, and some volatile oil pass to a condenser F. The soap powder is removed by a screw conveyer through a door 21. The oil and alkali may be separately sprayed into the chamber E, but are preferably pre-emulsified together. Sodium silicate, sodium carbonate, borax, sodium perborate, trisodium phosphate and heavy mineral oils may be added. Specification 504,118 is referred to.
154 Process and device for the distillation of glycerine and other materials containing impurities GB2357137 1937-08-27 GB500374A 1939-02-08
500,374. Distilling liquids. BAUDOT, J. Aug. 27, 1937, No. 23571. Convention date, Aug. 27, 1936. [Class 32] A process for distilling substances, such as glycerine, containing impurities, consists in heating the substance, converting it into a finely-divided form by subjecting it to reduction of pressure, mixing it with superheated steam, and passing the gaseous mixture through a series of condensers maintained at different temperatures for fractionally condensing the constituents. Apparatus for the purpose comprises a jacketed chamber 1 maintained under reduced pressure and provided with a spraying nozzle 6. 9 through which the glycerine &c. is fed to the chamber after passing through a heater 8. The nozzle is surrounded by a pipe 5 through which superheated steam from a heater 7 is admitted to the chamber to mix with the finely-divided glycerine. The mixture passes by pipe 16 to a condenser 16 where part is condensed and collects in a receiver 17, while the remainder passes by pipe 18 to a second condenser 19, where another fraction collects in a receiver 20. The residual vapours pass tb a heat exchanger 22 connected to a vacuum pump at 23.
155 Apparatus for distilling high boiling point liquids GB1230538 1938-04-25 GB492882A 1938-09-28
In a distillation vessel for high boiling-point liquids, the liquid space is divided by an annular partition into an inner and an outer chamber; liquid entering the inner chamber by a pipe a is heated by a steam coil c, and is kept in circulation by a steam jet w which raises it through the tube d until it is thrown back by a deflector plate z. A pipe spray g may also be used. The partially distilled liquid passes out through an aperture k into the outer chamber where it is further distilled as it progresses round from the entry k to the outlet e, separated by a partition m. Vertical guide plates n with base apertures v serve to secure an even passage of the liquid. The outlet e communicates through a valve s with the immersion pipe f, to permit re-circulation. A spray trap t3 is arranged to return liquid to the inner chamber. The annular partition q is preferably double, and may communicate with the vapour space, particularly when working under vacuum.
156 Process for the extraction of glycerin distillery slops and other industrial residues containing product FR829539D 1937-02-25 FR829539A 1938-06-29
157 Improvements in the distillation of glycerin GB65738 1936-12-01 GB486415A 1938-06-01
An apparatus for distilling glycerine and substances of similar physical properties comprises a still having closed steam heating surfaces to distil the glycerine, a boiler-condenser in which the heat of condensation of the glycerine generates steam, and means for drawing off condensed water from the closed steam heating surfaces and supplying it to the boiler. The apparatus described is for use in carrying out the process described in Specification 486,311. Glycerine is distilled in a still 1, Fig. 1, from which the mixed vapours of glycerine and water pass through a goose-neck 2 to a separator 3 which removes entrained liquid. The vapours pass on through a pipe 4 to a boiler-condenser 5 in which the heat of condensation of the glycerine is used to generate steam, part of which is utilized in the still. A pipe 6 conveys the water vapours, uncondensed glycerine and impurities to a condenser-concentrator 8, from which the water vapour and other volatile impurities are led off by a vacuum line 10. The still 1 is heated by steam coils 11, 12, 13, 14, 15, Fig. 2, controlled by inlet valves A, B, C, D, E on a steam pipe S. Condensed water is withdrawn through the valves a ... e and via a pressure-release trap 19, which prevents escape of steam, to a receiver 17. The reduction in pressure at the trap 19 to a lower pressure controlled by a valve 25, causes part of the hot water to vaporize in the receiver 17, and to pass as steam to a glycerine preheater 22. The water collecting in the receiver 17 passes through a cooler 28 to the boiler-condenser 5, whence the steam generated passes by pipe 31 to a superheater coil 16 in the still 1. High-pressure steam from the line S can also be supplied through a valve F to the coil 16, which is connected at its lower end to a ring manifold 35 carrying ejector jets 37 which cause effective circulation of the glycerine over the heating coils. Steam from line S is also supplied to perforated rings 41, 42, 43. The boiler-condenser, Fig. 5, is supplied with distilled water from the receiver 17 by an inlet pipe 29. Glycerine vapours entering at 4 pass through the tubes 56 containing twisted metal baffles 57; the condensed glycerine falls into a trough 58 and thence out by the pipes 59, 72 to the receiver 7. Uncondensed vapours pass out at 6 to the condenser-concentrator 8. The steam generated passes out by the pipe 31 to the still; a proportion may be lead off by pipe 52 for heating the condenser-concentrator 8. The condenser-concentrator, Fig. 6, contains banks of horizontal Field-tubes so arranged that the cooling water flows generally downward but locally upward to prevent accumulation of air in pockets. Thus water entering by a pipe 45 flows through a Field-tube 47 back to a space 46 connecting with a second Field-tube 48, situated above the first, and from which the water passes to a connection 50 leading down to the lower of the next pair of Field-tubes underneath, and so on, until it emerges by the pipe 75. The lowest two pipes are provided with steam from the pipe 52. Glycerine vapours enter at the bottom and proceed upwards, condensate forming on the pipes being collected in the tank 9.
158 Improvements in distillation of glycerin and in the distillation and purification ofother volatile substances GB3296936 1936-12-01 GB486311A 1938-06-01
Glycerine and similar volatile substance are distilled by heating the substance by indirect contact with saturated steam under pressure with resulting condensation of water from such steam and with vaporization of the glycerine, and then reducing the pressure on the condensed water and bringing it into indirect contact with the hot glycerine vapours to effect condensation of glycerine and generation of steam from the water at a lowered pressure, and passing steam so generated directly into the glycerine undergoing distillation to promote such distillation. Apparatus as described in Specification 486,415 is utilized in carrying out this method.
159 Improvements to the process for the manufacture of an anhydrous soap and glycerin FR828022D 1937-10-18 FR828022A 1938-05-09
160 Improvements in or relating to a process of and apparatus for making soap GB3266035 1935-11-25 GB471172A 1937-08-25
In a continuous process for the manufacture of soap, a stream of saponified material is released into a chamber in which a partial vacuum is maintained, glycerine is continuously removed from the chamber as vapour and molten or plastic soap is continuously withdrawn, or the vacuum is maintained by the continuous removal of glycerine vapour whilst the soap is maintained in the molten or plastic condition until its removal. Soap from cottonseed oil must be kept above 455 DEG F. and soap from palm oil or tallow above 518 DEG F., until it is removed from the chamber. As shown, tallow, cottonseed oil, or other glyceride is pumped from a tank 11, and aqueous potash or other saponifying agent from a tank 22, to a mixer 14. The pumps 1, 2 are driven through variable-speed gearing 18 set to deliver the materials in proper proportions. The mixture is saponified under pressure in the coil 4 and the resulting mixture of glycerine, steam, and soap is released through a nozzle 51 into a jacketed chamber 5 connected to barometric condensers 7 for the glycerine and 8 for the steam, and to a small vacuum pump 84. Superheated steam or hot inert gas may be admitted to the chamber 5 at 56. The soap, which is free from water, and is of low glycerine-content, is removed by a pump 6 driven by variable-speed gearing 43, and any desired proportion of water may be mixed with the outflowing soap by a pump 3. The soap is extruded at 97 by a screw-conveyer 94 driven by variable-speed gearing 95, and jacketed for cooling. The pump 6 may be dispensed with. If sufficient water is added to the soap, the extruded bar is a plastic solid, but if the proportion of water is less than about 12 per cent, a friable mass is produced which readily breaks into soap powder. Specification 396,769 is referred to.
QQ群二维码
意见反馈