Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
  • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
  • C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/24—Stationary reactors without moving elements inside
  • B01J19/2415—Tubular reactors
  • B01J19/2435—Loop-type reactors
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
  • B01J8/12—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by gravity in a downward flow

Definitions

• the present invention concerns a method and equipment for hydrogenating or hardening oil, fat and fatty acids by adding hydrogen and using a catalyst.
• a large, closed tank or container with a stirring device is used.
• the oil or fat is treated in batches by adding hydrogen in an eddy current which is created by a mechanical stirrer designed as a rotor with several sets of propeller blades or as a screw.
• reaction speed defined as the iodine reduction ( ⁇ I) per time unit is low, for example 0.3 ⁇ l/min.
• the consumption of hydrogen in the first half hour can be approximately 80 % of the total consumption, while it can take 4-6 hours for the hydrogenation to be completed.
• reaction speed in the Sullivan system is stated as 1.5 - 2 ⁇ I/min. , but apart from this improvement the weaknesses of the system are the same as for the conventional batch process.
• the aim has been to achieve higher reaction speed regular hydrogen consumption simple, reliable process control selective hydrogenation low catalyst consumption reduction of energy consumption (kW) .
• the stated objectives were achieved by a procedure for hardening oil or fat which is characterised by a semi-continuous or continuous process in which the catalyst is mixed with preheated fat or oil in a mixing device, whereby the mixture is passed through a preferably serpentine-like, vertically-mounted pipe loop or one or more static mixers for the addition of hydrogen and, possibly, inert gas so that a turbulent co-current flow is achieved, the mixture is cooled during hydrogenation and, possibly, the oil, catalyst, inert gas and excess hydrogen gas are recirculated after the hardening process.
• the present invention comprises processing equipment for the hardening of oil or fat which is characterised by feed and mixing devices for the addition and mixing of oil and a catalyst, a preferably serpentine-like, vertically-mounted pipe loop, or one or more static mixers and cooling devices with feed devices for hydrogen gas and, possibly, inert gas, and devices for collecting the oil, separating and recirculating any inert gas and the supply, separation and, possibly, recirculation of used hydrogen gas, as well as a possible separation and recirculation of the catalyst.
• Fig. 5 shows a continuous process equipment for the hardening or hydrogenation of oil or fat
• Fig. 2 shows alternative equipment which, for example, can be used as a retrofit in existing hydrogenation systems.
• the equipment comprises, as Fig. 1 shows, a feed and mixing device A) , a serpentine-like pipe loop B) , and devices C) for separating and recirculating a catalyst, supply and recirculation of any inert gas, and supply and recirculation of any excess hydrogen gas.
• the feed and mixing device A consists of a holding and recirculation tank 1 with a stirring device 2 for catalyst suspension, a heat exchanger 3 and a feed and stirring tank 4 for the oil or fat, and pumps 6, 7 with appropriate pipes 9, 10 for the transporta ⁇ tion of the oil and the catalyst suspension respectively to a mixing point 10 where the pipes 8, 9 meet.
• the catalyst is preferably of Ni, deposited on carriers of minerals or plastics in the form of grain-like particles and the purpose of the stirring device 2 in the tank 1 is to keep this suspension homogeneous and prevent the deposition of catalyst particles on the base of the tank.
• another purpose of the stirring device 5 is to keep a regular temperature in the oil or fat in the tank 4.
• the oil, fat or fatty acid, depending on what is to be hardened, is fed from a storage tank or similar (not shown) via pipes 8, first through a heat exchanger 3, where it is heated, and subsequently to the stirring tank 4. From tank 4 the oil can be recirculated through the heat exchanger 3 by means of the pump 6. During the hydrogenation process the oil is pumped from tank 4 on to the mixing point 10 where it is mixed with the catalyst suspension from the holding tank 1. From here the mixture is transported through a serpentine-like pipe loop 11 into the hydrogenation system B) . Hydrogen in the quantities required is supplied to the pipe loop 11 at several points 12 via supply pipes 13 and flows with the oil in a turbulent co-current (bubble-flow) , at the same time as the reaction with the oil takes place.
• a turbulent co-current bubble-flow
• any inert gas for example nitrogen, is added at different points 14 via supply pipes 15.
• any inert gas is intended to regulate the hydrogen cover of the catalyst and thereby control the reaction speed and obtain selective hydrogenation, at the same time as maintaining the turbulent gas-liquid current.
• coolers or heat exchangers 21 are mounted in the pipe loop. The purpose of these is to gradually remove the heat generated during the exothermic hardening process and keep the optimum reaction temperature. This heat can be expediently used to preheat untreated oil which is to be fed into part A) of the processing system. This produces a considerable reduction in energy consumption.
• the oil, catalyst and gas mixture goes to part C) of the processing system, which comprises a collection tank 16 with a stirring device 17, a pipe system 18 with a compressor 19 for recirculating the excess inert and hydrogen gas, as well as a pipe system 20, possibly with a centrifuge and/or filter or similar built in to separate and recirculate the catalyst slurry.
• the purpose of the stirring device 17 in the collection tank 16 is to prevent the catalyst being deposited on the base.
• the collection tank works like a gas separator and the collected gas is extracted from the top of the tank by means of the compressor 19.
• the gas which is extracted from the tank 16 may, depending on the reaction process, be pure inert gas or a mixture of inert gas and hydrogen and this gas is mixed with hydrogen from the hydrogen supply (not shown) via the pipe 18.
• the gas which is supplied to the pipe loop 11 through points 12 is thus a mixture of hydrogen and inert gas and the mixture ratio may, as stated earlier, be regulated in a precise manner to obtain the desired hardening speed and degree of hardening.
• the oil/catalyst mixture is fed from the base of the tank 16 and, possibly, through a centrifuge or similar.
• the hardened oil is fed to a storage tank (not shown) via the pipe 22 while the catalyst is fed back to the holding tank 1 via the pipe 23.
• a joint tank for the catalyst and oil may be used, whereby the catalyst is recirculated to tank 4 instead of tank 1.
• tank 4 instead of tank 1.
• Fig. 2 shows an alternative processing system in accordance with the present invention which can easily be used for converting conventional batch systems but which can also be used for new systems.
• This solution can be described as semi-continuous as the oil is fed into the autoclave or container 24 in batches while the actual hydrogenation takes place continuously.
• Fig. 2 shows a large, closed container 24 which is designed to contain a certain quantity of oil plus a calcu ⁇ lated quantity of catalyst, preferably Ni catalyst.
• a base stirrer ensures that the catalyst, which is mainly in the oil in the lower part of the container, is kept in suspension and is not deposited on the base of the container.
• the oil mixed with the catalyst is pumped out of the tank by means of a pump 26 via a pipe system 27 through a serpentine pipe system as described for the continuous hydrogenation system or through a set of static mixers/heat exchangers back to the top of the tank and out into it via a diffuser 29 which slows the speed and distributes the oil/gas flow.
• the hydrogenation takes place in exactly the same way as with a continuous system such as that described earlier. Excess hydrogen and inert gas are extracted from the top of the tank and recirculated as in the continuous system. In the system shown in Fig. 2 the tank has no built-in heating device.
• the heat exchangers in the combined static mixer/heat exchanger are used to heat up the oil in the container but as soon as the tempera ⁇ ture is sufficiently high (about 160°C) and the hardening process has started, the heat exchangers are used to cool the oil.
• Reference numbers 32 and 33 show, respectively, the inlet and the outlet for the heat exchanger's heat exchange medium which may be steam during heating and may be water during cooling.
• the catalyst particles will sink towards the base in such a way that the catalyst concentration will be highest in the area where the stirring takes place. Moreover, the stirring is concentrated in the base volume so that it does not affect the oil above (above the dotted line) . This means that the hardened oil which is returned to the container through the diffuser 29 will sink relatively quickly towards the base. In this way it will be possible to use a much smaller catalyst charge than with conventional batch systems.
• the oil can be pumped out and the container emptied through the discharge pipe 34. New, unhardened oil and catalyst are added to the container through the filling pipes 35, 36.
• Fig. 1 and Fig. 2 a serpentine- like pipe loop and static mixers were used respectively.
• the present invention is, however, not limited to these two examples as, instead of a pipe loop as shown in Fig. 1, static mixers may be used and, instead of the static mixers shown in Fig. 2, a pipe loop with separately arranged heat exchangers may be used.
• the length of the pipe loop or the number and length of the static mixers and heat exchangers can be adapted to the hydroge ⁇ nation process to give optimal operating conditions.
• the two examples shown are thus alternatives which are kept at the desired temperature by means of built-in heat exchangers/ coolers in the loop 8.
• Ni catalyst of type Pricat 9910 with 20 % Ni was used as the catalyst.
• the quantity corresponds to 0.04 % Ni in the oil which is the normal catalyst quantity when hardening soya oil in a batch reactor.
• the supply of hydrogen was 3 x 44 Nl/min. and the pressure in the pipe loop was 8 bar.
• the test was carried out over 45 minutes.
• the mean oil flow was 3.8 kg/min. and the mean dwell time for the oil in the pipe batch was 7 minutes.
• the so-called iodine value (IV) before hardening was measured at 129 and after hardening at 59.7, i.e. a difference of approxi ⁇ mately 70 ⁇ IV.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Fats And Perfumes (AREA)
• Catalysts (AREA)
• Lubricants (AREA)

Priority Applications (3)

Applications Claiming Priority (2)

Publications (1)

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Family Applications (1)

Country Status (7)

Cited By (1)

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Citations (5)

• 1992
  • 1992-11-12 NO NO924356A patent/NO176361C/no unknown
• 1993
  • 1993-11-11 PL PL30891093A patent/PL308910A1/xx unknown
  • 1993-11-11 EP EP94901074A patent/EP0674698A1/en not_active Withdrawn
  • 1993-11-11 WO PCT/NO1993/000167 patent/WO1994011472A1/en not_active Application Discontinuation
  • 1993-11-11 BR BR9307448A patent/BR9307448A/pt not_active Application Discontinuation
  • 1993-11-11 AU AU55782/94A patent/AU5578294A/en not_active Abandoned
  • 1993-11-11 CA CA 2149248 patent/CA2149248A1/en not_active Abandoned

Patent Citations (5)

Non-Patent Citations (1)

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