New method for removing nitrogen-containing compounds from a feedstock

Abstract

The invention relates to a new method for removing or reducing nitrogen-containing compounds from a raw material.

Description

Technical Field

[0001] This invention relates to the field of raw material processing and purification. Specifically, this invention addresses the problem of removing or reducing nitrogen-containing compounds from raw materials. The raw materials can be of any plant or animal origin and lipids derived therefrom. This invention also relates to purified raw materials obtainable by the method according to the invention. Background Technology

[0002] In this art, methods for purifying raw materials using various techniques are described. For example, WO 2018 / 024728 relates to a phase separation method for removing phosphorus compounds present in raw materials that may contain animal fats. Other compounds removed from the raw materials are metals, such as iron, magnesium, and calcium, or compounds containing these metals. Summary of the Invention

[0003] As described herein, the present invention relates to a method for removing or reducing nitrogen-containing compounds from raw materials.

[0004] Importantly, the method may include the following steps:

[0005] a) Provide raw materials containing lipids of plant or animal origin.

[0006] b) Add the acid and adsorbent together to the feedstock in a), and optionally add water.

[0007] c) Heat the mixture obtained in step b).

[0008] d) Separate the adsorbent from the mixture obtained in c).

[0009] e) Remove and / or neutralize the acid.

[0010] To obtain raw materials that are essentially free of nitrogen compounds or have a reduced nitrogen compound content.

[0011] In one aspect, the present invention relates to the removal or reduction of nitrogen-containing compounds from raw materials. The nitrogen-containing compound can, in principle, be any compound containing at least one nitrogen atom in its chemical formula, whether organic or inorganic. In one aspect, the nitrogen-containing compound can be an amine or an amide.

[0012] In another aspect, the nitrogen-containing compound removed from the raw material, or the nitrogen-containing compound whose content is reduced, can be any nitrogen-containing compound that is soluble in the raw material or the raw material matrix.

[0013] Raw materials can be of any plant or animal origin, and therefore can be based on any plant or any part of a plant, derivative or product, or any product derived from or based on algae or microbial oil.

[0014] The acid that can be used according to the invention can be any acid in principle. There are several non-limiting embodiments, such as, for example, sulfuric acid (H2SO4), hydrochloric acid (HCl), nitric acid (HNO3), phosphoric acid (H3PO4), boric acid (H3BO3), hydrofluoric acid (HF), hydrobromic acid (HBr), perchloric acid (HClO4) or hydroiodic acid (HI), or any combination or mixture thereof.

[0015] Other examples of acids that can be used include, for example, methanesulfonic acid.

[0016] According to the present invention, the adsorbent can, in principle, be any mineral-based adsorbent material. Mineral-based adsorbent materials can be in any form, such as, for example, solids, such as powders, granules, beads, or mixed with liquids, such as, for example, suspensions or gels. In one aspect, the adsorbent can be a silica-based compound. The silica-based compound can be any type of silica gel, which can be an amorphous and porous form of silica (silica), composed of an irregular three-dimensional framework of alternating silicon and oxygen atoms having nanoscale pores and voids. The pores can contain water or some other liquid, or can be filled with gas or a vacuum (also known as silica dry gel). In one aspect, any mineral-based adsorbent material can be used. In another aspect, the adsorbent can be amorphous silica, preferably Trisyl.

[0017] According to the invention, the heating in the method (step c) can be in any range, such as, for example, about 60°C to about 100°C, and preferably about 80°C.

[0018] According to this process, once the heating step is considered complete, the adsorbent can be removed or separated from the mixture. The removal or separation of the adsorbent can be achieved by filtration and / or centrifugation and / or precipitation. In one aspect, the removal of the adsorbent can be achieved by decantation.

[0019] According to the present invention, the process method may include neutralizing the acid used in the purification process. The process method may alternatively include any other methods for removing the acid used in the process method. In another alternative, neutralization and other removal methods may be employed. A non-limiting embodiment may be rinsing the obtained raw material with, for example, water or an aqueous solution. Neutralization can be carried out by any method known in the art and may include, for example, the addition of a suitable base / alkaline solution, such as, for example, the addition of a NaOH solution.

[0020] The purified feedstock obtained may be substantially free of any nitrogen-containing compounds, or may contain nitrogen-containing compounds in reduced amounts. As described herein, the purified feedstock may be substantially free of any nitrogen-containing compounds soluble in the feedstock, or may contain nitrogen-containing compounds soluble in the feedstock in reduced amounts. Such compounds may be, for example, amides or amide-containing compounds, or may be amines or amine-containing compounds, or any mixture thereof. Thus, the purified feedstock may be 100% free of any nitrogen-containing compounds, or may contain less than, for example, about 20%, or less than about 15%, less than about 10%, less than about 5%, less than about 3%, less than about 1%, less than about 0.5%, or less than about 0.1% of nitrogen-containing compounds, in wt%.

[0021] As described herein, the present invention relates to purified raw materials that can be obtained by the method according to the present invention.

[0022] definition

[0023] The term "feedstock" is intended to refer to any material based on or derived from any plant or animal source. It can also refer to any material based on algae, bacteria, or fungi. The term can also specifically include any vegetable oil, vegetable fat, animal fat and oil, and mold oil selected from, for example, rapeseed oil, canola oil, colza oil, tallow, sunflower oil, corn oil, technical / distillers corn oil, soybean oil, sesame oil, olive oil, linseed oil, cottonseed oil, mustard oil, palm oil, palm effluent sludge (PES), peanut oil, castor oil, coconut oil, animal fats (such as suet, tallow, blubber), alimentary fat, starting materials produced by genetic engineering, and biological starting materials produced by microorganisms such as algae, fungi, bacteria, yeast, etc., or any combination or mixture thereof.

[0024] The term "reduction" is intended to mean that the content of a component present in any material, such as, for example, a raw material, is lower than the content present in any material prior to any processing, or, for example, in a raw material used as a starting material or raw material in any process. Reduction can be a reduction of one or more components by 100%, and thus substantially complete removal, or a reduction of at least about 30%, such as, for example, a reduction of at least about 40%, such as, for example, a reduction of at least about 50%, such as, for example, a reduction of at least about 60%, such as, for example, at least about 70%, such as, for example, a reduction of at least about 80%, such as, for example, a reduction of at least about 85%, such as, for example, 90%, such as, for example, at least about 95%, such as, for example, at least about 97%, such as, for example, at least about 98%, such as, for example, at least about 99%. This percentage can be measured in weight % (wt%) or volume % (vol%).

[0025] In one aspect, the reduction in nitrogen-containing compounds is in the range of approximately 40% to approximately 60%.

[0026] The term "acid" is intended to refer to any Lewis acid or any compound capable of donating proton ions. Acids can be inorganic or non-inorganic, such as, for example, sulfuric acid (H₂SO₄), hydrochloric acid (HCl), nitric acid (HNO₃), phosphoric acid (H₃PO₄), boric acid (H₃BO₃), hydrofluoric acid (HF), hydrobromic acid (HBr), perchloric acid (HClO₄), or hydroiodic acid (HI), or, for example, methanesulfonic acid (CH₃SO₃H), or any combination or mixture thereof.

[0027] The term "silica-based" compound is intended to refer to any compound containing silica atoms. Such a compound can be a silica-based compound, such as, for example, a silica-based compound. Further examples are, for example, silica or silica degels of any form or construction. Further non-limiting examples are, for example, silica-alumina gels. Various silica-based compounds are commercially available, such as... These compounds are also included in the term. Detailed Implementation

[0028] As described above, the present invention relates to a method for removing or reducing nitrogen-containing compounds from raw materials.

[0029] This invention provides a method for utilizing raw materials used in the preparation of other raw materials, such as fuels and fine chemicals, thereby substantially removing or reducing undesirable nitrogen-containing compounds in the purified raw materials. Therefore, this invention provides a simple and efficient processing method for removing nitrogen-containing compounds from raw materials, and thereby provides a method for using renewable raw materials. The inventors of this invention have surprisingly discovered that, for example, when an adsorbent is added together with an acid in this process, particularly effective removal of nitrogen-containing compounds and / or phosphorus-containing compounds and / or metal-containing compounds can be observed. This is merely one of the many beneficial features of this invention, the details of which will be discussed below.

[0030] Furthermore, the method of the present invention allows for the large-scale industrial production of purified raw materials from renewable resources.

[0031] In one aspect, the method according to the invention may include the following steps:

[0032] a) Provide raw materials containing lipids of plant or animal origin.

[0033] b) Add the acid and adsorbent together to the raw material in a), and optionally add water.

[0034] c) Heat the mixture obtained in step b).

[0035] d) Separate the adsorbent from the mixture obtained in step c).

[0036] e) Remove and / or neutralize the acid.

[0037] This results in raw materials that are essentially free of nitrogen compounds or have a reduced nitrogen compound content.

[0038] In another aspect, the present invention may relate to a method comprising or consisting of the following steps:

[0039] a) Provide raw materials containing lipids of plant or animal origin.

[0040] b) Add about 0.5 wt% to about 5 wt% of acid and about 0.5 wt% to about 5 wt% of amorphous silica adsorbent to the raw material in a), and optionally add about 1 wt% to about 5 wt% of water.

[0041] c) Heating the mixture obtained in step b) to a temperature ranging from about 30°C to about 200°C over a period of about 5 minutes to about 6 hours.

[0042] d) Separate the adsorbent from the mixture obtained in c).

[0043] e) Remove and / or neutralize the acid.

[0044] This results in raw materials that are essentially free of nitrogen compounds or have a reduced nitrogen compound content, wherein the nitrogen compounds are compounds that are soluble in the raw materials or the raw material matrix.

[0045] In one aspect, step e) occurs after step d).

[0046] In one aspect, the method according to the invention can be performed sequentially, i.e., starting with step a), then step b), followed by step c), and step d), and finally step e).

[0047] In a further aspect, the method according to the invention does not include any step or reaction condition between one or more of steps a)-b)-c)-d) or -e).

[0048] The raw materials according to the invention can, in principle, be based on or derived from any material of any plant or animal origin. Therefore, the raw materials according to the invention can be used as starting materials or raw materials for the further production of any type of fuel or fuel component, and this can be used as a raw material / starting material for the production of renewable fuels. The raw materials can also be used for the production of any type of fine chemicals. Therefore, the raw materials can also be based on any algae, bacteria, or fungal material. Non-limiting embodiments may include any vegetable oil, vegetable fat, animal fat and animal oil, and mold oil selected from, for example, rapeseed oil, canola oil, rapeseed oil, tallow, sunflower oil, corn oil, technical corn oil / distilled corn oil, soybean oil, sesame oil, olive oil, flaxseed oil, cottonseed oil, mustard oil, palm oil, palm effluent sludge (PES), peanut oil, castor oil, coconut oil, animal fat (such as suet, tallow, whale blubber), recycled edible fat, used cooking oil, genetically engineered starting materials, and bio-starting materials produced by microorganisms such as algae and bacteria, or any combination or mixture thereof.

[0049] According to this process, once the raw material is provided, it is mixed or contacted with an acid or acidic compound (which may be present in step b of the process). According to the invention, the acid can in principle be any Lewis acid or a compound capable of providing or releasing hydrogen ions. Non-limiting examples include, for instance, any type of inorganic acid, such as, for example, sulfuric acid (H₂SO₄), hydrochloric acid (HCl), nitric acid (HNO₃), phosphoric acid (H₃PO₄), boric acid (H₃BO₃), hydrofluoric acid (HF), hydrobromic acid (HBr), perchloric acid (HClO₄), or hydroiodic acid (HI), or any mixture thereof.

[0050] In one respect, the inorganic acid can be sulfuric acid (H2SO4).

[0051] However, the acid according to the invention can also be any acid other than inorganic acids, such as, for example, any type of organic acid. Further non-limiting embodiments may include, for example, methanesulfonic acid (CH3SO3H) or ethanesulfonic acid (CH3CH2SO3H).

[0052] In one respect, the acid can be methanesulfonic acid (CH3SO3H).

[0053] In one aspect, acid is added in an amount of about 0.5 wt% to about 5 wt%, preferably about 1 wt% or about 2 wt%, based on the weight content of the raw material.

[0054] According to this process, the acid added to the feedstock can, in principle, be of any concentration, such as, for example, at least about 60 vol%, for example, at least about 70 vol%, for example, at least about 80 vol%, for example, at least about 85 vol%, for example, at least about 90 vol%, for example, at least about 95 vol%, for example, at least about 96 vol%, for example, at least about 97 vol%, for example, at least about 98 vol%, or for example, at least about 99 vol%, or for example, at least about 99.5 vol%. The acid can be provided in the form of an aqueous solution of a given concentration.

[0055] Acids can be mixed or brought into contact with raw materials by mechanical stirring or agitation. Alternatively, high-shear mixing can be employed.

[0056] Add the adsorbent to process step b). This addition must provide contact between the adsorbent and the acid / feed mixture. Contact or mixing can be achieved by mechanical stirring or agitation or high-shear mixing. The purpose of the adsorbent is to adsorb water-soluble nitrogen compounds from the acid / feed mixture.

[0057] Optionally, the acid is added to the raw material so that it can be fully mixed or contacted with the raw material, and mixed for a period of time of about 30 seconds to about 1 hour, such as, for example, about 30 minutes, such as, for example, about 20 minutes, such as, for example, about 15 minutes, such as, for example, about 10 minutes, such as, for example, about 5 minutes, such as, for example, about 3 minutes, such as, for example, about 1 minute.

[0058] In one aspect, once the acid is added to the raw material, it is mixed or stirred for a period of about 5 minutes before the silicon-based compound is added.

[0059] Optionally, the acid / raw material mixture is heated to a temperature above ambient temperature, such as, for example, about 30°C to about 200°C, such as, for example, about 40°C, such as, for example, about 50°C, such as, about 60°C, such as, for example, 70°C, such as, for example, about 80°C, such as, for example, about 90°C, such as, for example, about 100°C, such as, about 110°C, such as, about 130°C, such as, about 150°C, such as, about 170°C, such as, about 200°C.

[0060] In one aspect, the acid / raw material mixture is heated to a temperature of approximately 80°C before the adsorbent is added.

[0061] In another aspect, optionally, before being added and mixed with the adsorbent, the acid / raw material can be mixed by heating at any temperature above ambient temperature, such as, for example, about 30°C to about 200°C, such as, for example, about 40°C, such as, for example, about 50°C, such as, for example, about 60°C, such as, for example, about 70°C, such as, for example, about 80°C, such as, for example, about 90°C, such as, for example, about 100°C, such as, for example, about 110°C, such as, for example, about 130°C, such as, for example, about 150°C, such as, for example, about 170°C, such as, for example, about 200°C for a period of time of about 30 seconds to about 1 hour, such as, for example, about 30 minutes, such as, for example, about 20 minutes, such as, for example, 15 minutes, such as, for example, 10 minutes, such as, for example, 5 minutes, such as, for example, 3 minutes, such as, for example, about 1 minute.

[0062] Therefore, in one aspect, the acid / raw material mixture is heated to about 80°C for about 5 minutes before the adsorbent is added.

[0063] In one aspect, the acid and the adsorbent are added to the raw material essentially simultaneously and mechanically mixed or stirred together with the raw material. This mixing or stirring can take place over a period of time ranging from about 30 seconds to about 1 hour, such as, for example, about 30 minutes, such as, for example, about 20 minutes, such as, for example, about 15 minutes, such as, for example, about 10 minutes, such as, for example, about 5 minutes, such as, for example, about 3 minutes, such as, for example, about 1 minute.

[0064] The adsorbent can, in principle, be any mineral-based compound, preferably a silica-based compound. Silica-based compounds can, in principle, be any silica-based compound, such as, for example, silica-based compounds. A further non-limiting embodiment is, for example, a silica or silica degel of any form or configuration. A further non-limiting embodiment according to the invention is, for example, a silica-alumina gel. Various silica-based compounds are commercially available, such as, for example... These compounds are also included in this invention.

[0065] Based on the content of the raw material by weight, the adsorbent can be added in an amount of 0.5 wt% to about 5 wt%, preferably about 1 wt% or about 2 wt%.

[0066] The process according to the invention may optionally include the addition of water in step b), or in other words: in some aspects, the invention may include the addition of water, or in other aspects, the addition of any water in step b) may not be included. Based on the weight of the raw materials, the amount of water added in step b) is about 1 wt% to about 5 wt%, and preferably about 2 wt%.

[0067] According to the present invention, the process in step c) includes a heating step. Heating can be performed at any temperature above ambient temperature, such as, for example, in the range of about 30°C to about 200°C, such as, for example, in the range of about 35°C to about 150°C, such as, for example, in the range of about 40°C to 130°C, such as, for example, in the range of about 50°C to 120°C, such as, for example, in the range of about 60°C to about 100°C, such as, for example, in the range of about 70°C to about 90°C, or at temperatures of about 40°C, about 50°C, about 60°C, about 70°C, about 80°C, about 90°C, about 100°C, about 110°C, about 120°C, about 130°C, about 140°C, about 150°C, about 160°C, about 170°C, about 180°C, about 190°C, or about 200°C.

[0068] In one aspect, the heating in step c) can be in any temperature range from about 60 to about 100°C. In another aspect, the heating in step c) can preferably be about 80°C.

[0069] The heating in step c) can be carried out for any period of time from about 5 minutes to about 90 minutes, preferably about 20 minutes or about 60 minutes. Alternatively, it can be carried out for up to about 6 hours, such as, for example, up to about 5 hours, such as, for example, up to about 4 hours, such as, for example, up to about 3 hours, such as, for example, up to about 2 hours, such as, for example, up to about 90 minutes, such as, for example, up to about 80 minutes, such as, for example, up to about 70 minutes, such as, for example, up to about 60 minutes, such as, for example, up to about 50 minutes, such as, for example, up to about 40 minutes, such as, for example, up to about 30 minutes, such as, for example, up to about 20 minutes, such as, for example, up to about 10 minutes, such as, for example, up to about 5 minutes.

[0070] Heating step c) can be performed under reduced pressure. Reduced pressure can, in principle, be below atmospheric pressure (1 atm, corresponding to 1013.25 mbar), such as, for example, pressures of about 100 mbar to about 900 mbar, such as, for example, about 200 mbar to about 900 mbar, such as, for example, about 300 mbar to about 900 mbar, such as, for example, about 400 mbar to about 900 mbar, such as, for example, about 500 mbar to about 900 mbar, such as, for example, about 600 mbar to about 900 mbar, such as, for example, about 700 mbar to about 900 mbar, or preferably about 800 mbar.

[0071] Optionally, the drying step following step c) may include treating the mixture obtained in step c) at an elevated temperature. Such a temperature may be any temperature above ambient temperature, such as, for example, in the range of about 30°C to about 200°C, such as, for example, in the range of about 35°C to about 150°C, such as, for example, in the range of about 40°C to 130°C, such as, for example, in the range of about 50°C to 120°C, such as, for example, in the range of about 60°C to about 100°C, such as, for example, in the range of about 70°C to about 90°C, or temperatures of about 40°C, about 50°C, about 60°C, about 70°C, about 80°C, about 90°C, about 100°C, about 110°C, about 120°C, about 130°C, about 140°C, about 150°C, about 160°C, about 170°C, about 180°C, about 190°C, or about 200°C.

[0072] In one aspect, the drying step may include processing at a temperature of about 90 to about 110°C, preferably about 105°C.

[0073] Optionally, the drying step following step c) may also include treating the mixture under reduced pressure. Reduced pressure can, in principle, be below atmospheric pressure (1 atm, corresponding to 1013.25 mbar), such as, for example, at about 100 mbar to about 900 mbar, such as, for example, about 200 mbar to about 900 mbar, such as, for example, about 300 mbar to about 900 mbar, such as, for example, about 400 mbar to about 900 mbar, such as, for example, about 500 mbar to about 900 mbar, such as, for example, about 600 mbar to about 900 mbar. For example, at pressures of about 700 mbar-900 mbar or preferably about 800 mbar, or alternatively at least 90 mbar, such as at least 80 mbar, such as at least 70 mbar, such as at least 60 mbar, such as at least 50 mbar, such as at least 40 mbar, such as at least 30 mbar, such as at least 20 mbar, such as at least 10 mbar, such as at least 5 mbar, such as at least 1 mbar.

[0074] In one aspect, the pressure reduction can be about 50 mbar to about 100 mbar, or preferably about 80 mbar.

[0075] Optionally, the drying step following step c) can be carried out for any suitable period of time, or until it is considered sufficient to remove the required amount of water, or until the amount of water remaining in the mixture is considered acceptable. Such a period of time can be from about 5 minutes to about 90 minutes, preferably about 20 minutes or about 60 minutes. Alternatively, it can be up to about 6 hours, such as, for example, up to about 5 hours, such as, for example, up to about 4 hours, such as, for example, up to about 3 hours, such as, for example, up to about 2 hours, such as, for example, up to about 90 minutes, such as, for example, up to 80 minutes, such as, for example, up to about 70 minutes, such as, for example, up to about 60 minutes, such as, for example, up to about 50 minutes, such as, for example, up to about 40 minutes, such as, for example, up to about 30 minutes, such as, for example, up to about 20 minutes, such as, for example, up to about 10 minutes, such as, for example, up to about 5 minutes.

[0076] In one aspect, the time period can be any period from about 5 minutes to about 60 minutes, or preferably about 15 minutes or about 45 minutes.

[0077] Therefore, according to one aspect, the present invention can relate to a method comprising treating a raw material with an acid in an amount of about 1 wt% to about 2 wt% (relative to the weight of the raw material) and an adsorbent in an amount of about 2 wt% to about 4 wt% (relative to the weight of the raw material), optionally adding water in an amount of about 2 wt% to about 4 wt% (relative to the weight of the raw material), and heating the resulting mixture at about 80°C under reduced pressure of about 800 mbar for a period of about 20 minutes to about 60 minutes. Thereafter, the mixture may optionally be heated at about 105°C under reduced pressure of about 80 mbar for a period of about 15 minutes to about 45 minutes.

[0078] According to the invention, the adsorbent can be removed by any suitable method known in the art. In one aspect, the adsorbent is removed in step d), thereby separating the adsorbent from the mixture obtained in c).

[0079] The adsorbent can be separated by filtration, precipitation / sedimentation, centrifugation, or decantation, or any combination thereof. Optionally, it can be separated under vacuum or reduced pressure, such as, for example, at pressures below atmospheric pressure (1 atm, corresponding to 1013.25 mbar of standard atmospheric pressure), such as, for example, about 100 mbar to about 900 mbar, such as, for example, about 200 mbar to about 900 mbar, such as, for example, about 300 mbar to about 900 mbar, such as, for example, about 400 mbar to about 900 mbar, such as, for example, about 500 mbar to about 900 mbar, such as, for example, about 600 mbar to 900 mbar. For example, the removal of the adsorbent is carried out at a pressure of about 700 mbar to 900 mbar, or preferably about 800 mbar, or alternatively at least 90 mbar, such as at least 80 mbar, such as at least 70 mbar, such as at least 60 mbar, such as at least 50 mbar, such as at least 40 mbar, such as at least 30 mbar, such as at least 20 mbar, such as at least 10 mbar, such as at least 5 mbar, such as at least 1 mbar.

[0080] The acid added to the process can be removed from the treated mixture by any suitable means. According to the invention, the acid can be removed from the process in step e). In one aspect, the acid is removed by neutralization with a solution of an alkali / basic compound. In another aspect, the acid is removed by rinsing the mixture with, for example, water or a suitable aqueous solution. In yet another further aspect, the acid is removed by neutralization and rinsing.

[0081] The neutralizing agent can, in principle, be any suitable alkali, such as, for example, NaOH, KOH, Ca(OH)2, or aqueous solutions thereof. The aqueous solution can, in principle, have any concentration of alkali / alkaline compound to the extent that the final water content does not necessitate further removal of excess water in any subsequent process.

[0082] The concentration can be, for example, about 50 wt% or higher, such as, for example, 60 wt% or higher, such as, for example, 70 wt% or higher, such as, for example, 80 wt% or higher, etc.

[0083] According to the invention, relative to nitrogen-containing compounds present in the raw material prior to processing according to the method, the amount of nitrogen-containing compounds soluble in the raw material or raw material matrix can be reduced by at least about 20 wt%, such as, for example, about 30 wt%, such as, for example, about 40 wt%, such as, for example, about 50 wt%, such as, for example, 60 wt%, such as, for example, about 70 wt%, such as, for example, about 80 wt%, such as, for example, about 90 wt%, such as, for example, about 95 wt%, such as, for example, about 98 wt%, or at least substantially free of any nitrogen-containing compounds soluble in the raw material or raw material matrix. In one aspect, the nitrogen-containing compound can be an amine and / or an amide (such as, for example, phosphoramide) or any salt thereof.

[0084] According to the invention, the method is also capable of reducing phosphorus or phosphorus-containing compounds and / or any metals present in the raw materials prior to the processing / method according to the invention. According to one aspect of the invention, the amount of phosphorus or phosphorus-containing compounds and metals is removed by at least about 80%, such as, for example, at least about 85%, such as, for example, at least about 90%, such as, for example, about at least about 95%, such as, for example, at least 98%, or for example, at least 99% or more.

[0085] In one aspect, the invention also relates to raw materials that can be obtained by the method / process according to the invention.

[0086] Therefore, the present invention relates to purified raw materials wherein the amount of phosphorus-containing compounds is less than 5 ppm, such as, for example, less than 4 ppm, less than, for example, 3 ppm, less than 2 ppm, or less than 1 ppm.

[0087] In a further aspect, the present invention relates to purified feedstocks, wherein the amount of nitrogen-containing compounds comprising primary amides is less than about 900 ppm or less, such as, for example, about 800 ppm or less, such as, for example, about 700 ppm or less, such as, for example, about 600 ppm or less, such as, for example, about 500 ppm or less, such as, for example, about 250 ppm or less, such as, for example, about 100 ppm or less, such as, for example, about 50 ppm or less, such as, for example, about 30 ppm or less, such as, for example, about 10 ppm or less, such as, for example, about 5 ppm or less. In one aspect, the content of primary amides may be about 1.0 wt% or less (based on the weight of the purified feedstock), such as, for example, about 0.8 wt% or less, such as, for example, about 0.6 wt% or less, such as, for example, about 0.4 wt% or less, such as, for example, about 0.3 wt% or less, such as, for example, about 0.2 wt% or less, such as, for example, about 0.1 wt% or less.

[0088] In a further aspect, the metal content of the purified feedstock may be less than about 20 ppm or lower, such as, for example, about 15 ppm or lower, such as, for example, about 10 ppm or lower, such as, for example, about 5 ppm or lower, such as, for example, about 1 ppm or less.

[0089] The present invention also relates to the use of feedstocks obtainable by the method of the invention for the preparation of any type of fuel or for the preparation of fine chemicals. Therefore, the method according to the invention provides purified feedstocks obtained by the method, wherein the feedstocks meet various requirements for further processing into, for example, fuels. Such requirements may be, for example, sufficiently low impurity levels to allow any type of catalytic reaction to proceed without causing catalyst poisoning or hindering other reaction conditions.

[0090] Example

[0091] The invention is illustrated below by way of the following non-limiting embodiments.

[0092] Example 1

[0093] Heating animal fat feedstock with concentrated H₂SO₄ (e.g., 1 wt% or 2 wt%) for a set time, with or without a small amount of water (e.g., 2 wt% or 4 wt%), will result in a decrease in phosphorus, metals, total nitrogen compounds, and amides. Excess acid should be washed away by water extraction or neutralized with alkali.

[0094] As demonstrated in the following examples, a particularly effective treatment was found when Trisyl silica was added to the acid treatment:

[0095] Low-quality animal fat (P = 70 ppm, total metals Si, K, Mg, Ca, Al, Zn, Fe, Co = 344 ppm) was treated with sulfuric acid (2 wt%), water (4 wt%), and silica (Trisyl, 4 wt%) for extended periods under the following conditions (60 min, 80 °C, 800 mbar, then 45 min, 105 °C, 80 mbar). Trisyl was removed by filtration under vacuum. Excess sulfuric acid was neutralized by washing the oil with an aqueous solution of NaOH (50 wt%).

[0096] The new treatment removed 95% of phosphorus (from 70.3 ppm to 3.7 ppm) and 97% of metals (from 344 ppm to 10.6 ppm). Furthermore, the total nitrogen and primary amide content in the bleaching oil were reduced by 60% (total nitrogen from 1670 ppm to 715 ppm, and primary amides from 0.86 wt% to 0.36 wt%).

[0097] Example 2

[0098] Heating the lipid feedstock with concentrated H₂SO₄ (e.g., 1 wt% or 2 wt%) for a set time, with or without a small amount of water (e.g., 2 wt%), will result in a decrease in its nitrogen concentration, and as determined, the portion of the nitrogen removed is in the form of primary amides. Excess acid needs to be washed away or neutralized with alkali.

[0099] When Trisyl silica was added to acid treatment, a particularly effective treatment was found:

[0100] Tallow fatty acid distillate (TFAD) was mixed with sulfuric acid (1 wt%) and water (2 wt%), and amorphous silica, such as Trisyl 3000 silica (2 wt%), was added at 80 °C. The reaction mixture was stirred at 80 °C and 800 mbar for 20 minutes, and then at 105 °C and 80 mbar for 15 minutes. Silica was removed by filtration, and the oil phase was washed with water to remove residual acid. The phases were then separated by centrifugation. After treatment, the nitrogen content in the feed decreased from 1940 mg / kg to 795 mg / kg (-59%), while the primary amide content decreased from 1.09 wt% to 0.65 wt% (-40%).

[0101] Example 3

[0102] Heating PES (palm effluent sludge) feedstock with concentrated H2SO4 (e.g., 1 wt%) for a set time, with or without a small amount of water (e.g., 2 wt% or 4 wt%), will result in a decrease in P, metals, and total N. Excess acid needs to be flushed away or neutralized with alkali.

[0103] A particularly effective treatment was found when amorphous silica-based compounds such as Trisyl silica were added to the acid treatment:

[0104] PES was treated with sulfuric acid (1 wt%) and amorphous silica (2 wt%) for extended periods under the following conditions (60 min, 80 °C, 800 mbar + 45 min, 105 °C, 80 mbar). The concentrations were N = 90.4 ppm, P = 26.0 ppm, and total metals = 241.4 ppm. Trisyl was removed by filtration under vacuum. Excess sulfuric acid was neutralized by washing the oil with a 50 wt% aqueous solution of NaOH. The pH of the aqueous phase after washing was 4.3, thus no further washing with water to remove excess acid was required.

[0105] Strong acid treatment removed 94% of phosphorus (from 26 ppm to 1.5 ppm), 98% of metals (from 241 ppm to 4.1 ppm, excluding residual Na from the neutralization step), and 66% of nitrogen (from 90.4 ppm to 30.8 ppm). Notably, it reduced the difficult-to-bleach iron and calcium to 1 ppm or less, respectively.

Claims

1. A method for removing or reducing nitrogen-containing compounds, including amides and amines, from feedstocks derived from renewable resources, the method comprising: a) Provide raw materials containing lipids of plant or animal origin. b) Adding the acid along with the adsorbent to the raw material in a) wherein the adsorbent is an amorphous silica adsorbent in an amount of 0.5 wt% to 5 wt% based on the weight content of the raw material, and optionally adding water, wherein the acid is sulfuric acid (H₂SO₄) in an amount of 0.5 wt% to 5 wt% based on the weight content of the raw material. c) The mixture obtained in step b) is heated to a temperature ranging from 30°C to 200°C for a period of 5 to 90 minutes under reduced pressure ranging from 100 mbar to 900 mbar, below atmospheric pressure. d) Separate the adsorbent from the mixture obtained in c). e) Remove and / or neutralize the acid. To obtain a raw material that is substantially free of nitrogen-containing compounds including amides or has a reduced amount of nitrogen-containing compounds including amides, wherein the nitrogen-containing compounds are compounds soluble in the raw material or the raw material matrix.

2. The method according to claim 1, wherein the raw material is vegetable oil, vegetable fat, animal fat and animal oil.

3. The method according to claim 2, wherein the raw materials are selected from corn oil, rapeseed oil, canola oil, rapeseed oil, tallow, sunflower oil, soybean oil, sesame oil, olive oil, flaxseed oil, cottonseed oil, mustard oil, palm oil, palm effluent sludge, peanut oil, castor oil, coconut oil, lard, tallow, whale blubber, recycled edible fats, or any combination or mixture thereof.

4. The method according to claim 1 or 2, wherein the amorphous silica adsorbent is any type of silica gel or silica dry gel.

5. The method according to claim 1 or 2, wherein the heating in step c) is performed in the range of 35°C to 150°C above the ambient temperature.

6. The method according to claim 1 or 2, wherein the heating in step c) has a time period of 5 minutes to 80 minutes.

7. The method according to claim 1 or 2, wherein the heating in step c) is performed under reduced pressure below atmospheric pressure of 200 mbar to 900 mbar.

8. The method according to claim 1 or 2, wherein step c) is followed by a drying step, the drying step comprising one or more of the following: i) Apply a temperature 30°C to 200°C above ambient temperature. ii) Apply a pressure reduction of 1 mbar to 900 mbar below atmospheric pressure. iii) The duration of the drying step is a period of 5 minutes to 6 hours.

9. The method according to claim 1 or 2, wherein the acid is added in an amount of 1 wt% based on the weight content of the raw material.

10. The method according to claim 1 or 2, wherein the acid is added in an amount of 2 wt% based on the weight content of the raw material.

11. The method according to claim 1 or 2, wherein the adsorbent is added in an amount of 1 wt% based on the weight content of the raw material.

12. The method according to claim 1 or 2, wherein the adsorbent is added in an amount of 2 wt% based on the weight content of the raw material.

13. The method according to claim 1 or 2, wherein the amount of water optionally added in step b) is 1 wt%-5 wt%.

14. The method according to claim 1 or 2, wherein the amount of water optionally added in step b) is 2 wt%.

15. The method according to claim 1 or 2, wherein the adsorbent is removed by filtration, centrifugation, sedimentation or any combination thereof and optionally under vacuum or reduced pressure.

16. The method according to claim 1 or 2, wherein the acid is removed by washing with water and / or by neutralization with the addition of a suitable base selected from NaOH, KOH or Ca(OH)2 or a solution thereof.

17. The method according to claim 1 or 2, wherein the amount of nitrogen-containing compounds soluble in the raw material or raw material matrix is ​​reduced by at least 20 wt% relative to the nitrogen-containing compounds present in the raw material prior to the method treatment, or is at least substantially free of any nitrogen-containing compounds soluble in the raw material or raw material matrix.

18. The method of claim 1 or 2, wherein at least 95% of the amount of phosphorus and metal is removed.

19. A raw material obtainable by the method according to any one of claims 1-18.

20. Raw materials obtainable by the method according to any one of claims 1-18 for use in fuel preparation or for use in the preparation of fine chemicals.