EA036685B1 - Thermolytic fragmentation of sugars - Google Patents

Abstract

The invention concerns a process for large scale and energy efficient production of oxygenates from sugar in which a sugar feedstock is introduced into a thermolytic fragmentation reactor comprising a fluidized stream of heat carrying particles. The heat carrying particles may be separated from the fluidized stream prior to cooling the fragmentation product and may be directed to a reheater to reheat the particles and recirculate the heated particles to the fragmentation reactor.

Description

Scope of invention

The invention relates to a method for converting a sugar-based feedstock into a C1-C3 oxygenate product and a system suitable for carrying out this method. The method and system are suitable for industrial applications, and the method can be carried out as a large-scale continuous process.

Background to the invention

Biomass is of particular interest as a feedstock because of its potential to be used as an additive and as a possible substitute for petroleum as a feedstock in the production of industrial chemicals. In recent years, research has been carried out on the development of various technologies for the use of biomass. A significant part of biomass is carbohydrates, so there are various strategies for their effective use as a feedstock for the production of industrial chemicals. These strategies include various methods based on fermentation, pyrolysis, and various processes such as hydrogenolysis or hydroformylation or acid catalyzed dehydration.

Examples of chemicals derived from biomass include: natural gas substitutes, biofuels such as ethanol and biodiesel, browning materials for food, and industrial chemicals such as diols (ethylene glycol and propylene glycol), acids (lactic acid, acrylic acid, and levulinic acid) and a wide range of other important chemical intermediates (epichlorohydrin, isoprene, furfural and synthesis gas).

In the area of pyrolysis, research has focused on the use of solid biomass feedstock and other cellulosic materials for the production of the above chemicals.

Studies have been conducted on the possibility of using sugars as a raw material for the production of browning materials for food products that contain a large amount of glycolaldehyde (also called hydroxyacetaldehyde) as the main browning agent.

US Pat. No. 5,397,582 and related publication WO 92/17076 (Underwood) describe a process for producing liquid smoke for browning food products by adding sugar and / or starch to two alternative types of gas-solid contact reactors. One type of reactor is a downdraft reactor where sugar is contacted with a heating medium (eg sand) to produce pyrolysis products, and the other is an upward flow fluidized bed reactor. In the last reactor, the feedstock is introduced into the heat-conducting particles in the form of sand. During thermolytic fragmentation, product vapors are formed. The stream of product vapors and waste heat-conducting particles is transferred to two external cyclones, which are located in series, and the resulting vapor stream condenses. Thermally conductive particles, including char residues, are recycled from the first stage cyclone to the bottom of the fragmentation reactor. The residence time of the product vapors is 0.03-2 s, the fragmentation temperature is 400-1000 ° C, and the pyrolysis vapors are cooled to a temperature of less than 300 ° C in less than 0.6 s. The document does not disclose how heat is provided to heat the waste heat-conducting particles. As a result of pyrolysis in the specified device of powdered starch at a temperature of 550 ° C, a pyrolysis liquid is formed, in which half of the extracted organic substances is glycolaldehyde.

US 7,094,932 (Maerski) describes a method for preparing an ingredient for browning food products by thermolytic fragmentation of an aqueous solution of sugar, and in particular glucose, to obtain a pyrolysis product with a high concentration of glycolaldehyde. This method uses a dense fluidized bed of sand particles (also referred to as a bubble bed). A glucose solution containing 25-99% water is introduced into the reactor layer and the reaction is carried out at a temperature of 500-600 ° C. The suggested residence time in the reactor is 0.1-5 seconds. Heat is provided by electrical heating. Condensation of the gaseous reaction product occurs in the surface condenser. The mass yield of glycolaldehyde in the condensed liquid fragmentation product is at least 50 wt% of the sugar fed to the reactor. The liquid fragmentation product includes C ₁ -C ₃ oxygenate compounds including formaldehyde, glycolaldehyde, glyoxal, pyruvaldehyde, and acetol. The main product of this reaction is glycolic aldehyde, while the efficiency of carbon regeneration in the condensate was up to 85-89% of the amount of sugar supplied to the reactor. Example 6 of US Pat. No. 7,093,932 describes an upscaling according to this method by feeding a feedstock containing 50% dextrose monohydrate (glucose) at a feed rate of 7.3 kg / h into a larger plant of the type described above, as a result whereby the yield of glycolic aldehyde was 66%. The residence time in this system was 2-3 s, and the temperature was in the range of 530-560 ° C. Heat was still provided by electrical heating.

Document WO 2014/131764 describes a method for producing ketene from a sugar solution, according to which the sugar solution is subjected to pyrolysis in the presence of a fluidized material with an area

- 1,036685 surfaces up to 600 m ² / g at temperatures less than 700 ° C. The fluidized material is silicon dioxide and the residence time is 50-150 ms.

Both Underwood and Maersky proposed systems for the production of a glycolaldehyde-rich product by pyrolysis of sugars in a reactor using sand particles as heat transfer media and with short residence times to provide a high conversion rate of sugar to glycolaldehyde. Nevertheless, the proposed system can not be used for industrial conversion of sugars into a mixture of _C1-C3 oxygenates-rich glycol aldehyde by thermolytic fragmentation.

Fluidized bed reactors are used to treat a variety of feedstocks. Their operation can be carried out using various modes of fluidization. The choice of the preferred mode is made depending on the used feedstock and target product, because of this there are a large number of different configurations of fluidized bed reactors.

Several reactor configurations have been investigated to convert biomass to bio-oil by pyrolysis, for example, dense phase (i.e., bubbly fluidized bed) and diluted phase (i.e. riser) reactors, as well as radically different types of reactors, such as ablation reactors. pyrolysis.

Document WO 2012/115754 describes a pyrolysis process in which solid biomass, such as wood or other plant material, and a solid heat carrier such as sand are mixed at the bottom of an upflow reactor and subjected to pyrolysis conditions to produce an effluent pyrolysis. The pyrolysis effluent is fed to a cyclone separator where it is separated into (1) a solids-rich fraction containing solid char and a recirculated portion of the solid heat carrier and (2) a solids-depleted fraction containing pyrolysis products. Pyrolysis products include crude pyrolysis oil and other valuable chemicals such as carboxylic acids, phenolic resins and ketones. The solids-enriched fraction is fed to a reheat reactor containing a fluidized bed of thermally conductive particles, in which the solid char by-product is burned in the presence of an oxygen-containing gas, and a cooling medium is added to reduce the reheat reactor temperature. The reheated solid coolant is fed back to the riser pyrolysis reactor where the heat transfer particles in turn transfer heat to the pyrolysis reaction mixture to effect the pyrolysis reaction. The vaporous pyrolysis products are cooled and separated.

The fluidized bed can also be used for the catalytic or thermal cracking of hydrocarbons. Catalytic cracking can be carried out using a fluid catalytic cracking (FCC) process in which high boiling point petroleum fractions are converted to relatively lighter products such as gasoline. Examples of thermal cracking include a fluidized coking process that converts heavy oil fractions, i. E. pitch, to produce gas oil, or thermal cracking processes, in which naphtha is converted to ethylene and propylene. These cracking processes are mainly carried out in circulating fluidized bed systems.

One device that can be used to crack light and heavy FCC feeds is described in US Pat. No. 5,302,280 (Lomas). The described system comprises an riser reactor for cracking the feedstock using a catalyst. After cracking, the catalyst particles are separated from the vapors and transferred to a regenerator reactor, and the vapors are quenched. The catalyst particles are contacted with an oxygen-containing stream in a dense fluidized bed, resulting in the combustion of residual coke to provide heat to the catalyst and remove coke from the catalyst particles.

Accordingly, currently development of new uses of _C1-C3 oxygenates, thereby projected growth in demand for such products produce. Such oxygenate products can, for example, be used to produce ethylene glycol and propylene glycol by hydrogenating them (see, for example, WO 2016/001169) or purifying hydrogen sulfide as described in WO 2017/064267. However, various other uses can be envisaged. As far as we know, there are currently no systems or methods that can actually be used for thermolytic conversion of sugars into glycolic aldehyde rich mixtures in high yield on an industrial scale.

Thus, there is currently a need for highly effective and improved process for producing C1-C ₃ oxygenates from sugars, which could be used for large scale production, as well as in systems that can be used to implement such methods.

Summary of the invention

The present invention, having the purpose to receive the _C1-C3 oxygenates high purity with high yield and efficiency of environmentally sound sources, have found that methods and systems that are currently used to perform fragmentation thermolytic

- 2 036685 (pyrolysis) of raw materials from environmentally friendly sources, have various disadvantages, which makes them unsuitable for such use on an industrial scale.

The inventors have developed a method for the production of high purity C ₁ -C ₃ oxygenates on an industrial scale. This method involves thermolytic fragmentation of a sugar solution in a fragmentation reactor, in which a sugar solution is fed into a fluidized bed of heat-conducting particles and converted into a riser-type reactor, the main fraction of particles is removed from the product stream, followed by quenching the product stream, and the removed particles are transferred to the reheating reactor. for heating and recirculation of heated particles to the fragmentation reactor. This method is a highly energy efficient process that provides a high yield of C ₁ -C ₃ oxygenates. The inventors have also found that when the feedstock is sugar, heat from an external source is required to heat the thermally conductive particles, and that it is preferable to reheat in a separate reactor.

In accordance with one aspect of the present invention, there is provided a method for thermolytic fragmentation of sugar to produce C ₁ -C ₃ oxygenates, said method comprising the steps of:

a) feeding thermally conductive fluidizable particles to a fluidized bed fragmentation reactor containing a riser and suitable for thermolytic fragmentation and for fluidizing the particle stream at a feed rate sufficient to maintain a temperature of at least 250 ° C, for example at least 300, 350, 400 or 450 ° C, after thermolytic fragmentation has occurred and sufficient to obtain a fluidized stream of particles;

b) feeding a feedstock solution containing sugar into a fluidized particle stream to effect thermolytic fragmentation of sugar to obtain a fragmentation product with a high particle concentration; then

c) separating a fraction of particles from a fragmentation product with a high concentration of particles to obtain a fragmentation product with a low concentration of particles;

d) Quenching the fragmentation product with a low particle concentration by at least 50 ° C so that from the moment the feedstock is fed into the fluidizing stream containing particles until quenching, the average residence time of the gas formed is maximum 5 s, for example, maximum 3 s, for example a maximum of 2, 1, 0.8 or 0.6 s; and

e) recovery of the crude fragmentation product,

f) transferring the particles separated in step c) to a reheater for heating; and

g) recirculation of heated particles to the fragmentation reactor.

The advantage of this method is that it provides an energy efficient method for producing a crude fragmentation product with a high yield of C ₁ -C ₃ oxygenates and a low content of undesirable by-products. This is achieved through a combination of features of the invention, which include the use of a sugar solution as a feedstock, a high heat transfer rate, a short residence time of the vapor of the fragmentation product, primary removal of particles before quenching the vapor of the fragmentation product, quenching the vapor of the fragmentation product after the first separation and reheating. particles in an external reheater. The method provides high energy efficiency and can be used in large-scale production of C ₁ -C ₃ oxygenates, for example, for their further processing into ethylene glycol and propylene glycol. This method can be used in the continuous production of C ₁ -C ₃ oxygenates.

Heat-conducting particles are heated in a heater located outside the fragmentation reactor, and then they are fed into the fragmentation reactor, for example, by direct contact with hot gas in another reactor. The particles are heated to a temperature sufficient to transfer heat from the particle heater to the fragmentation reactor to provide sufficient heat transfer to the sugar solution to thermolytic fragmentation of the sugar and to produce a fragmentation product stream containing most of the C ₁ -C ₃ oxygenates. The flow of particles in the fluidized bed can be adjusted in accordance with the flow of the feedstock to provide the required amount of heat for the feedstock. Particles of materials with a high heat capacity require less mass flow than particles of materials with a lower heat capacity. In one embodiment, the particles obtained in step a) are fed to the fragmentation reactor at a mass flow rate of at least 10 kg / s, preferably at a mass flow rate of 10-1000 kg / s.

In the context of the present invention, the term “fragmentation product” means a vaporous stream resulting from thermolytic fragmentation of sugar. The term high particle concentration fragmentation product means the fragmentation product before the first particle separation that contains a large amount of particles, and the term low particle concentration fragmentation product means the fragmentation product after the first particle separation that contains fewer particles. The term crude fragmentation product means the effluent from the fragmentation reactor from which a portion of the particles have been removed.

Preferably, the particles are selected from the group of materials consisting of sand, silicon dioxide, glass, aluminum oxide, steel and silicon carbide.

- 3 036685

Preferably, the average particle size is 20-400 microns, for example 20-300, 20-200 or 20,100 microns.

A fluidized bed reactor is a reactor in which a bed of particles is present to be fluidized by a stream of fluidizing gas, which is generally fed at the bottom of the reactor. The fluidization state of the particles in such a bed is controlled depending on the speed and physical properties of the fluidizing gas stream in combination with the physical properties of the particles. It is generally considered that in the dense bed / turbulent bed / bubble bed, the superficial flow velocity of the fluidizing gas inside the reactor is 0.1-2 m / s. The superficial velocity of the fluidizing flow in the fast bed (riser / transfer reactor) inside the reactor is considered to be 3-22 m / s. However, the exact range of velocities depends on the physical properties of the particles and fluidizing gas and can be determined experimentally or calculated by methods known in the art.

In the present invention, thermolytic fragmentation is carried out in a fluidized bed reactor operating in a fast fluidization mode, that is, in an upflow reactor. In general, the riser is a vertically elongated reactor with a fluidization inlet, a particle inlet, and a feed inlet at the bottom, with the particle inlet located along downstream of the fluidization flow inlet, and the feed inlet located downstream of the particle feed port. For the purposes of the present invention, the particles can form a dense phase fluidized bed in the region between the particle feed inlet and the feed inlet. If necessary, it is possible to dispense with the fluidization flow and therefore without an inlet for feeding the fluidization flow. For example, the feedstock can be supplied directly after the heat transfer particles and thus act as a fluidization stream.

The temperature of the particles at the feed of the particles to the fragmentation reactor is preferably at least 300 ° C, for example at least 400, 450, 500, 550, 600 or 650 ° C.

Preferably, the feed temperature of the particles is in the range 300-800 ° C, for example in the range 400-800 or 450-650 ° C.

The feedstock can be supplied at any time after the introduction of thermally conductive particles. When the raw material comes into contact with heat-conducting particles, an evaporation zone is formed, in which the solvent evaporates, and as a result of sugar fragmentation, the formation of gaseous products begins. This leads to an increase in the surface velocity of the gas, which as a result traps the heat-conducting particles. Accordingly, after the feed opening, the heat conductive particles and the feed form a fast layer above the evaporation zone, which can be called a riser. In accordance with one embodiment of the invention, the feed inlet is provided at the bottom of the riser.

In accordance with one embodiment of the invention, the fragmentation reactor comprises a first particle separator downstream of the riser for separating a particle fraction from a high particle concentration fragmentation product. The first particle separator may also be referred to as the end of the riser when it is located immediately after the riser. When the first particle separator is located before the cooling or quenching step of the fragmentation product stream, the advantage is that it eliminates the need to cool the heat-conducting particle fraction during cooling of the fragmentation product stream, thereby avoiding unnecessary heat loss.

In accordance with one embodiment of the invention, a major portion of the thermally conductive particles are separated in a first particle separator. Accordingly, in the first particle separator, more than 50 wt.% Of heat-conducting particles are separated from the fragmentation product with a high concentration of particles, for example, at least 60, 70, 80, 90, 95 or 99 wt.%. Preferably, the first particle separator is a reversing separator. In this type of separator, a rapid separation of the fragmentation product from the particles occurs, which allows quicker quenching and, thus, heat acts on the fragmentation product for a minimum time, thereby the amount of disintegrating fragmentation product is reduced, and further reaction of the oxygenate mixture in the fragmentation product is prevented ... The rapid heating of the feedstock and the rapid cooling of the fragmentation product thus ensured are highly preferred, since the average time period during which the oxygenates in the fragmentation product are exposed to heat and hence warm decomposition is very short, with the majority of the sugar being fed to the reactor, is subjected to sufficient heating for thermolytic fragmentation to occur.

Accordingly, the average residence time of the gas from feeding the feedstock to quenching is in the range of 0.01-5 s, for example 0.01-3 s, 0.1-1 s, or 0.3-0.8 s. The average residence time in the riser required for the majority of the sugar fed to the reactor to be exposed to sufficient heat to cause thermolytic fragmentation depends on the heat transfer rate of the particles. The heat transfer rate depends on factors such as the temperature of the feed particles, the heat capacity of the particles, the solvent used in the sugar solution, etc. Particle velocity and reactor design can be adjusted to provide sufficient, but not excessive, heat for thermolytic fragmentation. With this device, a very high heating rate of the feedstock can be achieved, in excess of 1000 ° C per second. The advantage of separating the heat-conducting particles from the fragmentation product with a high particle concentration, before quenching, is that in this way the residual heat of the heat-conducting particles can be regenerated.

In accordance with one embodiment of the invention, the gaseous product from the fragmentation reactor is separated from the particles before they enter the reheater. This can further increase product yield.

In accordance with one embodiment of the invention, the reactor comprises a downstream quenching step downstream of the first particle separator. The advantage of quenching after separation of the heat-conducting particle fraction is that it reduces energy losses. This increases the energy efficiency of the method. In addition, when fewer heat-conducting particles are present, the quenching of the fragmentation product stream is faster and requires less energy to be transferred. Preferably, the quenching is carried out by feeding a liquid, such as water or recycle streams from subsequent stages of the fragmentation reactor process, to the fragmentation product with a low particle concentration. Such a liquid can be an intermediate or a final product obtained after thermolytic fragmentation. This further increases the energy efficiency of the process. Alternatively, quenching can be accomplished by indirect heat exchange or by introducing colder particles into the low particle concentration fragmentation product. Preferably, the particles are of the same type as the particles used as heat-conducting particles, only at a lower temperature. The advantage of this is that when the particles are fed, they can form part of the recirculated particle stream. The liquid can be injected or sprayed into the fragmentation product with a low concentration of particles, for example, through nozzles in the fragmentation reactor.

In accordance with one embodiment of the invention, the quenching of the low particle concentration fragmentation product is carried out to a temperature of less than 450 ° C, for example less than 400, 350 or 300 ° C.

Thermolytic fragmentation of sugar is an endothermic reaction, mainly due to the evaporation of the feedstock. Thus, the heat-conducting particles will lose some heat during the process unless additional heat is supplied to the process. In accordance with one embodiment of the invention, the temperature difference between the particle feed temperature and the outlet temperature of the fragmentation reactor is in the range of 10-600 ° C, for example 50-250 ° C. In accordance with another embodiment of the invention, the temperature of the thermally conductive particles at the outlet of the fragmentation reactor is in the range of 250-700, for example 300-600 or 350-550 ° C.

The heat-conducting particles, separated in the first particle separator from the fragmentation product with a high concentration of particles, are transferred to a re-heater, in which the heat-conducting particles are heated with their subsequent recirculation to the fragmentation reactor. The advantage of such external heating of the heat-conducting particles is that the heat source does not affect the thermolytic fragmentation reaction. Thus, it allows for a heating process that involves combustion in the presence of excess oxygen to provide heat to initiate an endothermic reaction without oxygen affecting sugar peroxidation.

In accordance with one embodiment of the invention, the reactor includes a heating chamber for heating heat-conducting particles and a heating source. In accordance with one embodiment of the invention, the reheater is a fluidized bed reactor containing a riser.

Preferably, the temperature of the heat-conducting particles leaving the reheater is in the range of 300-800 ° C, for example 400-800, 400-700, or 500-700 ° C.

The fragmentation reactor may include a second particle separator located downstream of the quenching step. It is used to remove the remaining heat-conducting particles to obtain a fragmentation product of higher purity. Removing the maximum amount of particles reduces wear on downstream equipment and reduces the potential for disruption in subsequent steps. In the context of the present invention, the term to remove means to reduce the amount. In addition, the separated heat-conducting particles can be fed to the reheater. Alternatively, the heat-conducting particles removed in the second separator and which have been cooled can be further cooled and used as quench particles in the fragmentation reactor.

An advantage of using thermally conductive particles to provide heat for thermolytic fragmentation is that the fragmentation reactor may not contain a device.

- 5 036685 for heating neither inside nor on the surface of the reactor. However, this does not mean that the fragmentation reactor cannot contain such heating devices in principle. The use of particles to provide heat for thermolytic fragmentation of sugar is beneficial for several reasons. For example, the particles have a large surface area to transfer heat to large amounts of sugar. These advantages continue to exist even when using the method in large-scale production. In fact, it is unlikely that sufficient heat transfer will limit the throughput of the process according to the invention.

The feedstock solution obtained in step c) contains sugar. In accordance with one embodiment of the invention, the feed solution is an aqueous sugar solution. In the context of the present invention, the term sugar means a carbohydrate containing one or more C6 and / or C5 saccharide residues, mainly in the form of mono- and / or disaccharide (s). In accordance with one embodiment of the invention, the sugar is selected from the group consisting of sucrose, lactose, xylose, arabinose, ribose, mannose, tagatose, galactose, glucose and fructose, or mixtures thereof. Sugar can also be in the form of a sugar syrup. Thermolytic fragmentation of glucose provides a high yield of glycolaldehyde. Accordingly, if a high yield of glycolaldehyde is desired, sugars containing glucose residues are preferred.

In yet another embodiment of the invention, the feedstock solution is introduced into the fluidized bed reaction chamber as an aqueous solution containing up to 90 wt% sugar. In yet another embodiment of the invention, the feed solution is introduced into the fluidized bed reaction chamber as an aqueous solution containing 10-90 wt% sugar, eg 30-80%, or 40-70 wt% sugar.

The C ₁ -C ₃ oxygenates obtained using the method according to the present invention consist mainly of formaldehyde (C1), glycolaldehyde (C2), glyoxal (C2), pyruvaldehyde (C3) and acetol (C3). However, for most applications, C2 and C3 oxygenates are the most valuable product as a product. The crude fragmentation product obtained using the method of the present invention contains a mixture of C ₁ -C ₃ oxygenates. In this document the following terms may be used interchangeably: a mixture of C ₁ -C3 oxygenates, C ₁ -C3 product oxygenates and C ₁ to C ₃ oxygenates. In one embodiment, the fragmentation product contains a large amount of glycolic aldehyde, which means that at least 50%, for example at least 60% or 70% by weight of the mixture of C ₁ -C 3 oxygenates is glycolaldehyde. In yet another embodiment, at least 50%, for example at least 60, 70 or 80% by weight of the mixture of C ₁ -C 3 oxygenates is glycolaldehyde or glyoxal. In yet another embodiment, at least 3%, for example at least 5% or 7% by weight of the mixture of C ₁ -C 3 oxygenates is pyruvaldehyde. In yet another embodiment, at least 3%, for example at least 5% or 7% by weight of the mixture of C ₁ -C 3 oxygenates is pyruvaldehyde or acetol.

The method of the present invention can be used in the large-scale production of C ₁ -C ₃ oxygenates. Accordingly, the amount of sugar that can be processed by the present method is more than 1000 tons / year in one reactor, for example, more than 5000, 10,000, 50,000, 100,000 or 1,000,000 tons / year in one fragmentation reactor based on dry weight of sugar.

An advantage of the method and device according to the present invention is that they can provide a total carbon yield of C ₁ -C ₃ oxygenates of more than 60 mol%, for example, more than 70, 75 or 80 mol%. Since C ₂ and C ₃ oxygenates are generally more valuable than C ₁ oxygenates, it is desirable to provide high yields of C ₂ -C ₃ oxygenates. In accordance with one embodiment of the invention, the total carbon yield of C2-C3 oxygenates is greater than 60 mol%, for example, greater than 70, 75 or 80 mol%. According to yet another embodiment of the invention, the total carbon yield of C ₂ oxygenates is greater than 50 mol%, for example, greater than 60, 70, 75 or 80 mol%. According to yet another embodiment of the invention, the total carbon yield of the glycolaldehyde is greater than 50 mol%, for example, greater than 60, 70, 75 or 80 mol%.

In accordance with one aspect of the present invention, the reheater is a riser reactor (also referred to as a riser). An advantage of using this type of reheater is that large quantities of particles can be rapidly heated and that the combustion reaction can be carried out separately from heating the heat-conducting particles. The conductive particles are fed through the particle feed inlet and are heated within the reheater riser. The heated particles leave the reheater riser through the reheater outlet. Preferably, the temperature of the thermally conductive particles leaving the reheater is in the range 400-800 ° C, for example 500-700 ° C. The heated heat-conducting particles are circulated from the particle outlet from the reheater to the particle feed inlet to the fragmentation reactor. Heat-conducting particles are moved through the pipeline from the outlet for removing particles from the fragmentation reactor to the inlet for feeding particles into the re

- 6 036685 heater. In one embodiment, the particle outlet from the fragmentation reactor is located higher than the particle feed inlet to the reheater so that gravity will aid in transporting the particles. Likewise, heated particles are transferred through a conduit from the reheater particle outlet to the particle inlet to the fragmentation reactor. In one embodiment, the particle outlet from the reheater is located higher than the particle feed inlet to the fragmentation reactor so that gravity will aid in transporting the particles. An advantage of using a riser in both a fragmentation reactor and a reheater is that a circulating fluidized bed system can be used in which the particles rise within the riser and then gravity aids in the circulation of the particles between the two riser systems. This is a great advantage when commercially produced mixtures of C ₁ -C ₃ oxygenates from sugars.

To ensure a high carbon yield, it is desirable that the process produces a minimum amount of coke or char. However, with low levels of coke and semi-coke, there is a reduction in the amount of heat generated by the combustion of such by-products. When carrying out the method according to the present invention, it is possible to reduce the amounts of coke and char obtained. This requires the supply of heat from an external source. In accordance with one embodiment of the invention, the reheater includes an inlet for feeding fuel and combustion air, a burner, an inlet for feeding particles to a reheater, a reheater riser, a reheater particle separator, an outlet for venting gas from the reheater, and an outlet to remove particles from the reheater. The combustion air can be, for example, atmospheric air or other oxygen-containing gas.

Heat can be provided using a burner that is located inside the reheater and which burns the fuel in the presence of combustion air. Combustion gas from the combustion chamber may be fed to the bottom of the reheater riser where it is mixed with heat conductive particles to form a fluidization stream within the reheater riser.

In accordance with one embodiment of the invention, combustion of air and fuel takes place in a separate combustion chamber. The hot combustion gas can then contact the particles within the reheater riser, causing the particles to absorb heat from the combustion gas. The fact that the combustion chamber is separate from the particle feed inlet to the reheater has the advantage that higher thermal efficiency and lower emissions of unburned hydrocarbons can be achieved in this way.

Staged burners for combustion of fuel and air are known to those skilled in the art, which are used to reduce nitrogen oxide emissions. Such burners can also be used to carry out the present invention. Other ways to reduce NOx emissions are, for example, recirculating a portion of the exhaust gas from the reheater gas outlet to the burner section to reduce the oxygen content in the flame zone, or staging fuel and particulates into the reheater riser to create zones where the temperature and the oxygen content is lower and therefore to reduce the formation of nitrogen oxides.

Suitable fuels are, for example, natural gas, oil, coal, pyrolysis gas, gas from the gasification process, gases containing hydrogen and carbon monoxide, waste products and biomass. The advantage of using a gaseous fuel is that it does not contain ash, hence avoiding the problems associated with ash, such as fluidized bed agglomeration, which is often observed when using, for example, biomass fuels in solid form. In accordance with one embodiment of the invention, the preferred fuel is natural gas. Natural gas is a more readily available fuel and combustion is relatively environmentally friendly compared to other fuels. The combustion temperature is quite high. Consequently, the combustion in the combustion chamber can preferably be carried out separately from the reheater riser, and the supply of combustion gas to the reheater riser can be carried out in such a way as to provide the desired outlet temperature of the heated particles.

In accordance with one embodiment of the invention, excess oxygen from the reheater is separated from the particles before they enter the fragmentation reactor. This can further increase product yield and product purity by minimizing O2 oxygenate side reactions in the fragmentation reactor. The particle removal chamber is preferably located downstream of the reheater particle separator but upstream of the particle feed inlet to the fragmentation reactor.

In accordance with one embodiment of the invention, the thermolytic fragmentation process is carried out as a continuous process. This is an advantage in industrial applications.

In accordance with one embodiment of the invention, the thermolytic fragmentation process is carried out under an inert atmosphere, such as nitrogen or steam.

In accordance with one aspect of the present invention, there is provided a method for preparing a C ₁ -C ₃ hydroxy compound from sugar, said method comprising the steps of:

carrying out the thermolytic fragmentation process of the present invention to form a crude fragmentation product containing C ₁ -C ₃ oxygenates;

and then hydrogenating the crude fragmentation product to give the corresponding _{1 to} Ο ₃ hydroxy compounds. C ₁ -C ₃ hydroxy compounds are, for example, ethylene glycol, propylene glycol and methanol.

The process of the present invention can be carried out in a fragmentation reactor in which the thermally conductive particles are in a fluidized bed, and in which effective separation of particles after thermolytic fragmentation and effective reheating of the thermally conductive particles is achieved.

Accordingly, according to the present invention, there is provided a system for fragmentation of a sugar-based composition to produce C ₁ -C ₃ oxygenates, the system comprising a fragmentation reactor, said reactor comprising the following elements:

riser;

first particle separator;

an inlet for feeding a fluidization stream;

particle feed inlet;

feed inlet;

outlet for removal of particles;

outlet for product removal;

the riser is located inside the fragmentation reactor in its lower part;

the inlet for feeding the fluidization stream and the inlet for feeding the particles are located at the bottom of the riser;

the feed inlet is located at the bottom;

a riser above the particle feed inlet;

the riser is configured to fluidize the particles;

the first particle separator is located in the upper part of the riser and is configured to separate at least part of the particles from the fluidization stream, and the reactor further comprises a cooling section located downstream of the first particle separator, while said cooling section is configured to cool the flow fluidization leaving the first particle separator, and the system further comprises a reheater for reheating the particles leaving the fragmentation reactor, and the reheater comprises an inlet for feeding fuel and combustion air, a burner, an inlet for feeding particles to the reheater, a reheater riser, a reheater particle separator, an outlet for removing gas from the reheater, and an outlet for removing particles from the reheater.

The advantage of such a device is that it can carry out the method according to the present invention, which provides an energy efficient method for producing a crude fragmentation product with a high yield of C ₁ -C ₃ oxygenates, and a high carbon yield in the fragmentation product, thus using the specified the device provides a method that can be used for large scale production of, for example, ethylene glycol and propylene glycol from sugars. This device can be used in the continuous production of C ₁ -C ₃ oxygenates.

In accordance with one embodiment of the invention, the system may further comprise a second particle separator within the reactor, the second particle separator being located at the top of the fragmentation reactor and configured to further separate a fraction of particles from the fluidization stream.

In accordance with one embodiment of the invention, the quenching in the cooling section is performed by introducing liquid into the fragmentation reactor.

In accordance with one embodiment of the invention, the quenching in the cooling section is performed by feeding a stream of particles at a lower temperature to the fragmentation reactor.

In accordance with one embodiment of the invention, the cooling section comprises an indirect heat exchanger.

In accordance with one embodiment of the invention, the first particle separator is a small volume separator.

In accordance with one embodiment of the invention, the first particle separator comprises at least one reversing separator.

In accordance with one embodiment of the invention, the first particle separator comprises at least one tube, which is positioned such that one end thereof is hydraulically connected to the top of the riser and the other is directed downward and hydraulically connected to the fragmentation reactor, wherein it resides inside the fragmentation reactor and extends outside the riser.

In accordance with one embodiment of the invention, the second particle separator is at least one cyclone.

In accordance with one embodiment of the invention, the burner and the fuel and combustion air inlet are located downstream of the reheater riser, and the reheater inlet is located at the bottom of the reheater riser downstream of the burner, and the reheater inlet the reheater feed port is hydraulically connected to the reheater outlet, the reheater riser being configured to reheat the particles leaving the fragmentation reactor using gas heated in the burner.

In accordance with one embodiment of the invention, a reheater particle separator is located downstream of the reheater riser, and an outlet for withdrawing particles from the reheater is hydraulically connected to the particle feed inlet to the fragmentation reactor.

In accordance with one embodiment of the invention, a burner is provided in the combustion chamber. It can be clamped away from the riser. For example, the cross-sectional area of such a constricted portion is at least 25% less than the cross-sectional area of the higher riser, and the length of the constricted portion is at least 0.5 m.

Brief Description of Drawings

Examples of embodiments of the present invention will be explained with reference to the accompanying drawings. It should be understood that the accompanying drawings illustrate only examples of embodiments of the present invention and, therefore, should not be construed as limiting the scope of the present invention, as the invention may include other alternative embodiments of the invention.

FIG. 1 is a cross-sectional side view of a fragmentation reactor in accordance with one embodiment of the invention.

FIG. 2 is a top view of a fragmentation reactor in accordance with the embodiment depicted in FIG. one.

FIG. 3 is a cross-sectional view of a reheater in accordance with one embodiment of the invention.

FIG. 4 is a cross-sectional view of a system comprising a fragmentation reactor that is hydraulically coupled to a reheat heater, in accordance with one embodiment of the invention.

Item numbers:

1. Fragmentation reactor.

2. Fragmentation reactor riser.

3. First particle separator.

4. Second particle separator.

5. Cooling section.

6. Inlet for fluidizing flow.

7. Inlet for feeding particles.

8. Inlet for feeding raw materials.

9. Product outlet.

10. Particle outlet.

11. Reheater.

12. Inlet for fuel and combustion air.

13. Combustion chamber.

14. Inlet for feeding particles into the reheater.

15. Riser reheater.

16. Separator for reheater particles.

17. An outlet for removing particles from the reheater.

18. Outlet for venting gas from reheater.

19. Second reheater particle separator.

20. Particle removal chamber.

21. Fluidizing gas inlet to reheater.

22. Second inlet for feeding fluidizing gas and stripping gas to reheater.

Detailed description

As shown in FIG. 1 and FIG. 4, the fragmentation reactor of the invention is vertically extended. The riser 02 is made inside the fragmentation reactor, which has a small cross-sectional area relative to its height. This ensures a short residence time of the particles inside the riser. At the bottom of the riser there is an inlet 06 for supplying fluidizing gas,

- 9 036685 which is designed to supply fluidizing medium to the riser and port 07 for feeding particles. The fluidizing medium promotes movement of particles from the particle feed port to the feed port toward the top of the riser. In addition, the fluidization stream can be used to pretreat the particles before the particles contact the feedstock. The feed inlet 08, located above the particle feed and fluidization inlet, provides feed to the riser. In the illustrated embodiment, the feed inlet is located at the bottom of the riser, but its position may vary depending on process requirements.

Once the feedstock and particles have interacted in the riser, they are separated at the outlet of the riser in a first particle separator 03. In accordance with one embodiment of the invention, the first particle separator provides rapid separation of particles from the fragmentation product, since such rapid separation is an advantage. for a fashion. Thus, the particle separator can be a short residence time separator. In accordance with the embodiment shown in FIG. 2 and FIG. 3, the first particle separator comprises outlet pipes that are initially directed upward as the flow enters from the riser, and then they change direction by 180 °, and become directed downward within the fragmentation reactor, while they are outside the riser; in the context of the present invention, such a separator is referred to as a reversing particle separator. In accordance with the embodiment shown in FIG. 4, the first particle separator comprises a gas particle separator that enhances the exit of gas and solids from the riser in the tangential direction (relative to the wall of element 1) into the vessel 1; as a result, separation takes place. Part of the particles after leaving the first particle separator settles in the lower part of the fragmentation reactor. Accordingly, the described riser features, the position of the feed port and the short residence time in the first particle separator provide short contact times between particles and feed, which also depends on process parameters such as volumetric flow rate and equipment dimensions, which must all be adapted. to process requirements.

Cooling section 05 is located inside the fragmentation reactor above the first particle separator, next to it. In accordance with the present embodiment, the cooling section includes a quenching step in which a cooling medium such as water or a recirculation stream is injected, which rapidly and efficiently cools the product by evaporation. Other options may also be used in the cooling section, such as quenching by introducing a particle stream or using indirect heat exchangers, which can reduce the overall energy consumption of the fragmentation reactor system. Rapid product cooling can be essential to the process to achieve high yields as the product can be sensitive to prolonged exposure to elevated temperatures.

After cooling, the product is withdrawn from the fragmentation reactor through the product outlet 09. In the embodiment shown in FIG. 1 and FIG. 4, an additional second particle separator 04 is provided in the fragmentation reactor, which is intended to further separate the particle fraction from the product stream before withdrawing the product. In this section of the fragmentation reactor, the product is already cooled, therefore the residence time is less important. A second particle separator is provided, for example a cyclone, wherein said second particle separator provides a higher separation efficiency than a reversing separator alone (item 03). The gas outlet of the cyclone is connected to the product outlet, and the particles from the cyclone outlet are fed to the bottom of the fragmentation reactor (01), where they are kept in a fluidized state using the fluidization gas inlet (21). The cross-sectional distribution of the fluidizing gas is achieved, for example, by means of diffusers. In the lower part of the fragmentation reactor, waste particles are removed through an outlet 10 to remove particles, which are then fed to another reactor for reheating.

FIG. 2 is a top view of a fragmentation reactor in accordance with the embodiment depicted in FIG. 1, and in accordance with the description for the embodiment above. As shown, the riser is located at the center of the horizontal cross-section of the fragmentation reactor. In addition, a plurality of outlet pipes are shown that form a first particle separator as well as a second particle separator that is located away from the center of the fragmentation reactor.

FIG. 1 and FIG. 2, a second particle separator is located inside the fragmentation reactor. The second particle separator may contain one or more cyclones. In accordance with other embodiments not shown, these cyclones can also be located outside the fragmentation reactor, for example, above the fragmentation reactor, with dip tubes extending through the roof of the fragmentation reactor, or to the side of the fragmentation reactor with inclined dip tubes, or they can use, for example, a loop seal or an L-valve. If the second cyclones

- 10 036685 are placed outside the reactor vessel, the residence time of the oxygenate product in the fragmentation reactor can be reduced. In the embodiment shown in FIG. 4, external cyclones are placed on the fragmentation reactor.

FIG. 3 and FIG. 4 shows a reheater 11 for reheating particles leaving the fragmentation reactor. The inlet 14 for feeding particles into the reheater is hydraulically connected to the outlet 10 for removing particles from the fragmentation reactor, and the outlet 17 for removing particles from the reheater is hydraulically connected to the inlet 7 for feeding particles into the fragmentation reactor. The reheater further comprises a riser-type fluidized bed, a reheater riser 15 with a combustion chamber 13 that is hydraulically connected to the bottom of the riser. Through the inlet 12 for supplying fuel and combustion air, fuel and combustion air are supplied to the burner, during the operation of which heat is supplied to the riser of the reheater. The reheater inlet is located at the bottom of the reheater riser whereby particles leaving the fragmentation reactor enter the reheater riser where they are fluidized in an upward flow with hot gas supplied from the combustion chamber when heated. ... The connection between the burner and the particle feed inlet to the reheater is designed to reduce / prevent the escape of particles from the riser into the combustion chamber. This design can be implemented in various ways. FIG. 3 and FIG. 4 shows the pinch between elements 13 and 15, this pinch provides an increase in the gas velocity, which reduces / prevents the precipitation of particles. After reheating, the particles are separated from the combustion gas and fed back to the fragmentation reactor. In the embodiment shown in FIG. 3, the reheater particle separator 16 is a cyclone that removes gas from the reheater through the reheater gas outlet 18, with the separated particles exiting the reheater through the reheater particle outlet, which is connected to an outlet for removing particles from the cyclone of the reheater. It should be understood that the degree of separation in particle separators depends on various process parameters known to those skilled in the art, such as pressure drop across the separator, flow rate, particle size, etc.

In the embodiment shown in FIG. 4, the first particle separator is similar to element 03 of the fragmentation reactor. In embodiment 4, the system is also equipped with a second cyclone type particle separator (19). Both particle separators feed particles into the lower part of element 11. At the bottommost part of element 11 is a section (20) for removing fluidized particles from excess O ₂ . Distribution is carried out along the entire cross-section of the streams entering through the second inlets (22) for supplying fluidizing gas and stripping gas for elements 11 and 20 in accordance with the embodiment shown in FIG. 4, using diffusers or using other methods. Element 11 in FIG. 4 additional fluidizing gas inlets may be present, but are not shown. In addition, it is envisaged to strip off the gaseous product immediately before or after element (10) in FIG. 4.

Example

Example 1. Obtaining a mixture of C ₁ -C ₃ oxygenates, rich in glycolaldehyde, by thermolytic fragmentation of a sugar solution.

Fragmentation of the aqueous glucose solution was demonstrated in a riser type reactor setup. The particle feed inlet was located in front of the feed inlet. The surface gas velocity in the riser was approximately 6 m / s. The length of the upflow reactor was 6.2 m with an internal diameter of 41 mm. Two cyclones are located downstream of the riser, and the separated solids enter an external reactor for reheating. The residence time of the fragmentation product was approximately 1 second from the feed port to the first particle separator.

To collect the gaseous product, a portion of the gas stream leaving the second cyclone was fed to a condensation system. The liquid product quickly condensed by indirect cooling at 1 ° C and separated from the permanent gases. The constant gas flow was measured using a variable section flow meter.

The concentration of oxygenates in the liquid product was determined by HPLC, and the yield was calculated assuming that 8 wt% of the feed was lost with constant gases due to incomplete condensation of water, i.e. using a mass balance of 92%. This is considered to be a conservative but educated guess based on previous experience.

Based on this conservative assumption, approximately 60% of the carbon fed to the reactor was obtained as glycolaldehyde by thermolytic fragmentation of a 45 wt% glucose solution at approximately 500 ° C. Soda glass balls were used as the layer material.

- 11 036685

Embodiments of the invention

Embodiment 1

A method for thermolytic fragmentation of sugar to obtain Q-C3 oxygenates, said method comprising the following steps:

a) providing heat-conducting particles suitable for fluidization;

b) providing a fluidized bed fragmentation reactor containing a riser and suitable for thermolytic fragmentation and suitable for fluidizing the particle stream;

c) providing a feedstock solution containing sugar;

d) feeding the particles into the reactor at a feed rate sufficient to maintain a temperature of at least 250 ° C, such as at least 300, 350, 400 or 450 ° C, after thermolytic fragmentation has occurred and sufficient to produce a fluidized particle stream ;

e) feeding the feedstock into a fluidized particle stream to provide thermolytic fragmentation of sugar to obtain a fragmentation product with a high particle concentration; then

f) separating a fraction of particles from a fragmentation product with a high concentration of particles to obtain a fragmentation product with a low concentration of particles;

g) Quenching the fragmentation product with a low particle concentration by at least 50 ° C so that from the moment the feed is fed into the fluidization stream containing particles until quenching, the average residence time of the gas is a maximum of 5 seconds, for example, a maximum of 3 seconds, for example , maximum 2, 1, 0.8 or 0.6 s;

h) obtaining a crude fragmentation product;

i) transferring the particles separated in step f) to a reheater for heating; and

j) recirculation of the heated particles to the fragmentation reactor.

Embodiment 2

The method according to embodiment 1 of the invention, characterized in that the fragmentation product with a low concentration of particles passes through a second separation of particles after step g), in which there is a sharp cooling of the fragmentation product with a low concentration of particles, and before step h), in which obtaining a crude product of fragmentation.

Embodiment 3

A method according to any one of embodiments 1 or 2 of the invention, characterized in that the reactor in the lower part comprises an inlet for feeding particles and an inlet for feeding a raw material, while the inlet for feeding a raw material is located downstream of the opening for feeding particles.

Embodiment 4

The method according to embodiment 3, characterized in that the reactor in the lower part further comprises an inlet for supplying a fluidization stream, the inlet for supplying a fluidization stream being located in front of the inlet for feeding particles.

Embodiment 5

A method according to any one of embodiments 3 or 4 of the invention, characterized in that the particles form a dense phase fluidized bed in the region between the particle feed inlet and the feed inlet.

Embodiment 6

A method according to any one of embodiments 3-5 of the invention, characterized in that the feed inlet is located at the bottom of the riser.

Embodiment 7

A method according to any one of embodiments 1-5 of the invention, wherein the reactor comprises a first particle separator downstream of the riser.

Embodiment 8

A method in accordance with embodiment 7 of the invention, characterized in that the reactor comprises an in-process quenching step downstream of the first particle separator.

Embodiment 9

A method according to embodiment 8 of the invention, characterized in that the reactor, after the quenching step, comprises a second particle separator.

Embodiment 10

A method according to any one of embodiments 1-9 of the invention, characterized in that the reactor does not comprise heating means other than heat-conducting particles.

Embodiment 11

A method according to any one of embodiments 1-10 of the invention, characterized in that the sugar is a mono- and / or disaccharide.

Embodiment 12

A method in accordance with any of embodiments 1-11 of the invention, characterized in

- 12 036685 that the raw material solution contains an aqueous solution of sugar selected from the group consisting of sucrose, lactose, xylose, arabinose, ribose, mannose, tagatose, galactose, glucose and fructose; or mixtures thereof.

Embodiment 13

A method according to any one of embodiments 1-12 of the invention, characterized in that the sugar concentration in the feedstock solution is in the range of 10-90 wt%.

Embodiment 14

A method according to any one of embodiments 1-13 of the invention, characterized in that the temperature of the particles at the feed of the particles to the fragmentation reactor is preferably at least 300 ° C, for example at least 400, 450, 500, 550, 600 or 650 ° C.

Embodiment 15

A method according to any one of embodiments 1-14 of the invention, characterized in that the feed temperature of the particles is in the range of 300-800 ° C, for example in the range of 400-800 or 450-650 ° C.

Embodiment 16

A method according to any one of embodiments 1-15 of the invention, characterized in that the particles are selected from the group of materials consisting of sand, silicon dioxide, glass, alumina, steel and silicon carbide.

Embodiment 17

A method according to any one of embodiments 1-16 of the invention, characterized in that the average size of the heat-conducting particles is 20-400 microns, for example 20-300, 20-200 or 20,100 microns.

Embodiment 18

A method according to any one of embodiments 1-17 of the invention, characterized in that the particles obtained in step a) are fed into the fragmentation reactor at a mass flow rate of at least 10 kg / s.

Embodiment 19

A method in accordance with any one of embodiments 1-18 of the invention, characterized in that the velocity in the fragmentation reactor riser above the feed inlet is greater than 2 m / s, for example 3-22 m / s or 5-20 m / s ...

Embodiment 20. A method according to any one of Embodiments 1-19, wherein the reheater comprises an inlet for feeding fuel and combustion air, a burner, an inlet for feeding particles to a reheater, a reheater riser, a particle separator reheater, an outlet for exhausting waste gas from the reheater, and an outlet for removing particles from the reheater.

Embodiment 21. A method according to any one of Embodiments 1-20, characterized in that the temperature of the particles at the exit from the outlet for removing particles from the reheater is in the range of 300-800 ° C, for example in the range of 400-800 , 400-700 or 500-700 ° C.

Embodiment 22

A method according to any one of embodiments 20 or 21, characterized in that the burner is installed within a combustion chamber that is separate from the reheater riser and the combustion gas from the combustion chamber is supplied to the reheater riser.

Embodiment 23

A method according to any one of embodiments 20-22, characterized in that a portion of the waste gas from the reheater, after particle removal, is fed back to the combustion chamber.

Embodiment 24

A method according to any one of Embodiments 1 to 23 of the invention, characterized in that excess oxygen is separated from the particles before they are transferred from the reheater to the fragmentation reactor.

Embodiment 25

A method for producing a Ci-C3 hydroxy compound from sugar, said method comprising the following steps: carrying out a process in accordance with any of embodiments 1-24 of the invention; and then the crude hydrogenation product of fragmentation, to produce the corresponding _C1-C3 hydroxy.

Embodiment 26

A system for fragmentation of a sugar-based composition to obtain C ₁ -C ₃ oxygenates, comprising a fragmentation reactor, said reactor comprising the following elements: a riser; first particle separator; an inlet for feeding a fluidization stream; particle feed inlet; feed inlet; outlet for removal of particles;

- 13 036685 outlet for product removal; the riser is located inside the fragmentation reactor in its lower part; and the inlet for feeding the fluidization stream and the inlet for feeding the particles are located at the bottom of the riser; the feed inlet is located at the bottom of the riser; fluidizing the particles over the particle feed inlet in the riser; the first particle separator is located in the upper part of the riser and is configured to separate at least part of the particles from the fluidization stream, and the fragmentation reactor further comprises a cooling section located downstream of the first particle separator relative to the gas flow, while said cooling section is made with the possibility of cooling the fluidization stream leaving the first particle separator, and the system further comprises a reheater for reheating the particles leaving the fragmentation reactor, and the reheater comprises an inlet for feeding fuel and combustion air, a burner, an inlet for feeding particles into the reheater, reheater riser, reheater particle separator, reheater gas outlet and reheater particle outlet.

Embodiment 27

A system in accordance with embodiment 26, characterized in that the fragmentation reactor further comprises a second particle separator inside the fragmentation reactor, the second particle separator being located in the upper part of the fragmentation reactor and configured to further separate the particle fraction from the fluidization stream.

Embodiment 28

A system in accordance with any of embodiments 26 or 27, characterized in that the cooling section is capable of quenching by introducing liquid into the fragmentation reactor.

Embodiment 29

The system in accordance with any of the options 26 or 27 of the invention, characterized in that the quenching in the cooling section is carried out by feeding a stream of particles with a lower temperature into the fragmentation reactor.

Embodiment 30

A system in accordance with any of embodiments 26 or 27, wherein the cooling section includes an indirect heat exchanger.

Embodiment 31

A system in accordance with any of embodiments 26-30, wherein the first particle separator is a small volume separator.

Embodiment 32

A system in accordance with any one of embodiments 26-31 of the invention, wherein the first particle separator comprises at least one reversing separator.

Embodiment 33

A system in accordance with any one of embodiments 26-32 of the invention, characterized in that the first particle separator comprises at least one pipe, which is located such that one end thereof is hydraulically connected to the top of the riser, and the other is directed downward and hydraulically connected with a fragmentation reactor, while it goes beyond the riser.

Embodiment 34

A system in accordance with any one of embodiments 27-33 of the invention, wherein the second particle separator is at least one cyclone.

Embodiment 35

A system in accordance with any one of Embodiments 26-34, wherein the burner and the reheater fuel and combustion air inlet are located downstream of the reheater riser, and the reheater particle inlet is located at the bottom of the reheater riser downstream of the burner, and the inlet for feeding particles to the reheater is hydraulically connected to the outlet for withdrawing particles from the fragmentation reactor, while the reheater riser is configured to reheat particles leaving the fragmentation reactor using gas combustion from the combustion chamber.

Embodiment 36

A system according to any one of Embodiments 26-35, wherein a reheater particle separator is located downstream of the reheater riser and an outlet for removing particles from the reheater is hydraulically connected to an inlet for feeding particles into the fragmentation reactor ...

Embodiment 37

A system in accordance with any one of embodiments 26-36 of the invention, wherein the burner is located in a separate combustion chamber.

- 14 036685

Embodiment 38

A system in accordance with any embodiment 37 of the invention wherein the combustion chamber is pinched from the riser.

Embodiment 39

A system in accordance with any of embodiments 26-38, wherein the particle removal chamber is located downstream of the reheater particle separator but upstream of the particle feed inlet to the fragmentation reactor.

Claims (24)

CLAIM 1. A method for thermolytic fragmentation of sugar to obtain Q-C3 oxygenates, said method comprising the following steps: a) feeding thermally conductive fluidizable particles to a fluidized bed fragmentation reactor containing a riser and suitable for thermolytic fragmentation and for fluidizing the particle stream at a feed rate sufficient to maintain a temperature of at least 250 ° C after thermolytic fragmentation has occurred and sufficient to obtaining a fluidized stream of particles; b) feeding a feedstock solution containing sugar into a fluidized particle stream to effect thermolytic fragmentation of sugar to obtain a fragmentation product with a high particle concentration; then c) separating a fraction of particles from a fragmentation product with a high concentration of particles to obtain a fragmentation product with a low concentration of particles; d) quenching the fragmentation product with a low particle concentration by at least 50 ° C, so that from the moment the feedstock is fed into the fluidization stream containing the particles to quenching, the average residence time of the resulting gas is maximum 5 seconds; e) recovery of the crude fragmentation product, f) transferring the particles separated in step c) to a reheater for heating; and g) recirculation of heated particles to the fragmentation reactor. 2. The method according to claim 1, characterized in that in step a) the temperature is maintained at a temperature of at least 300, 350, 400 or 450 ° C. 3. A method according to claim 1, characterized in that in step d) the average residence time of the gas is at most 3, 2, 1, 0.8 or 0.6 s. 4. A method according to any one of claims 1 to 3, characterized in that the feed inlet is located at the bottom of the riser. 5. A method according to any one of claims 1 to 4, characterized in that the reactor comprises a first particle separator downstream of the riser. 6. A method according to claim 5, wherein the reactor comprises a quenching step downstream of the first particle separator. 7. A method according to any one of claims 1 to 6, characterized in that the sugar is a mono- and / or disaccharide. 8. The method according to any one of claims 1 to 7, characterized in that the feedstock solution contains an aqueous solution of sugar selected from the group consisting of sucrose, lactose, xylose, arabinose, ribose, mannose, tagatose, galactose, glucose and fructose; or mixtures thereof. 9. A method according to any one of claims 1 to 8, characterized in that the sugar concentration in the feedstock solution is in the range of 10-90 wt%. 10. A method according to any one of claims 1 to 9, characterized in that the temperature of the particles at the particle inlet to the fragmentation reactor is preferably at least 300 ° C, for example at least 400, 450, 500, 550, 600 or 650 ° C. 11. A method according to any one of claims 1 to 10, characterized in that the reheater comprises an inlet for feeding fuel and combustion air, a burner, an inlet for feeding particles to the reheater, a reheater riser, a reheater particle separator, an outlet for removing waste gas from the reheater; and an outlet for removing particles from the reheater. 12. A method according to any one of claims 1-11, characterized in that the temperature of the particles at the exit from the outlet for removing particles from the reheater is in the range of 300-800 ° C, for example, in the range of 400-800, 400-700 or 500-700 ° C. 13. A method according to any one of claims 11 or 12, characterized in that the burner is installed inside a combustion chamber that is separate from the reheater riser and the combustion gas from the combustion chamber is fed into the reheater riser. 14. A method according to any one of claims 1 to 13, characterized in that the excess oxygen is separated from the particles prior to their transfer from the reheater to the fragmentation reactor. 15. A method of obtaining 0 / -03 hydroxy compounds from sugar, including the implementation of the method - 15 036685 according to any one of claims 1-14; and then hydrogenating the crude fragmentation product to give the corresponding C ₁ -C ₃ hydroxy compounds. 16. A system for fragmentation of a sugar-based composition to obtain C ₁ -C ₃ oxygenates, comprising a fragmentation reactor, said reactor comprising the following elements: riser, first particle separator, fluidization inlet, particle inlet, feed inlet, particle outlet, product outlet, with the riser located inside and at the bottom of the fragmentation reactor ; and the inlet for feeding the fluidization stream and the inlet for feeding the particles are located at the bottom of the riser; the feed inlet is located at the bottom of the riser above the particle inlet; the riser is configured to fluidize the particles in the riser; and the first particle separator is located in the upper part of the riser and is configured to separate at least a portion of the particles from the fluidization stream, and wherein the fragmentation reactor further comprises a cooling section located downstream of the first particle separator, wherein said cooling section is configured cooling the fluidization stream leaving the first particle separator, and the system further comprises a reheater for reheating the particles leaving the fragmentation reactor, and the reheater comprises an inlet for feeding fuel and combustion air, a burner, an inlet for feeding particles into the reheater, a reheater riser a reheater particle separator, an outlet for venting gas from the reheater, and an outlet for venting particles from the reheater. 17. The system according to claim 16, characterized in that the cooling section is capable of quenching by introducing liquid into the fragmentation reactor. 18. The system of claim 16 or 17, wherein the first particle separator is a small volume separator. 19. A system according to any one of claims 16-18, characterized in that the first particle separator comprises at least one separator with a change in flow direction. 20. The system according to any one of claims 16-19, characterized in that the burner and the inlet for supplying fuel and combustion air to the reheater are located upstream of the reheater riser, and the inlet for feeding particles to the reheater is located in the lower portions of the reheater riser downstream of the burner, and an inlet for feeding particles to the reheater is in fluid communication with an outlet for removing particles from the fragmentation reactor, wherein the reheater riser is configured to reheat particles leaving the fragmentation reactor using gas burning from the burner. 21. The system according to any one of claims 16 to 20, characterized in that the reheater particle separator is located downstream of the reheater riser, and an outlet for removing particles from the reheater is connected downstream with an inlet for feeding particles into the fragmentation reactor ... 22. A system according to any one of claims 16-21, characterized in that the burner is located in a separate combustion chamber. 23. The system of claim 22, wherein the combustion chamber is separated from the riser by a pinch. 24. A system as claimed in any one of claims 16 to 23, wherein the particle removal chamber is located downstream of the reheater particle separator but upstream of the particle feed inlet to the fragmentation reactor.