BR112019010104A2 - production of dispersants for solid suspensions from vinasse-type materials - Google Patents

Abstract

A method for producing a dispersant for mineral suspensions comprising the steps of: (a) providing a vinasse-like material as input; b) passing the input through at least one nanofiltration step so as to separate the input into a retentate phase and at least one filtrate phase; c) collect the retentate phase previously obtained and supply it as a dispersant.

Description

PRODUCTION OF DISPERSANTS FOR SOLID SUSPENSIONS FROM VINHAÇA MATERIALS

Technical Field [0001] The invention relates to a method for producing a dispersant for mineral suspensions, a dispersant that can be obtained by this method and a method for producing a mineral suspension. In addition, the invention relates to a mineral suspension comprising a dispersant and a molded body that can be obtained by hardening a mineral binder composition.

State of the art [0002] Dispersants for mineral suspensions are widely used in the construction industry. Dispersants are used, in particular, as plasticizers or water reducing agents for hydraulic grip compositions, such as mortars and concrete. The water reducing agents allow to reduce the amount of water that is used to prepare hydraulic handle compositions without negatively affecting the rheological properties or workability of the hydraulic handle compositions. In addition, thanks to the reduced water fraction, the resistance of hardened mortars or concrete can be improved.

[0003] The most effective dispersing agents for hydraulic binders, such as cement or plaster, are substances produced synthetically, such as condensates of naphthalene sulfonic acid-formaldehyde, condensates of sulphonated formaldehyde melamine and polycarboxylates or polycarboxylate ethers. However, all of these substances are based on fossil raw materials, such as oil or natural gas.

[0004] Lignosulfonates are used as an alternative to the synthetic dispersants mentioned above. Lignosulfonates are natural waste from the paper and cellulose industry that use a pulping process for wood sulfite. In contrast to dispersants

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2/25 produced in the synthetic form mentioned above, lignosulfonates are waste products based on renewable raw materials.

[0005] Recently, dispersants derived from modified renewable materials, based, for example, on cellulose or starch, have also been proposed as dispersants.

[0006] In addition, other raw materials based on renewable materials can be added to the concrete water reducer, which provide some water reduction or are used to adjust the setting time. Such suitable materials are products derived from hydrolyzed cellulose or starch, such as glucose / corn syrups (with varying amounts of glucose, oligo and polysaccharides), glucose, gluconate, hydrogenated glucose products or waste products such as vinasse (production of bioethanol, citric acid or yeast) or molasses (from sugar production). Other types of sugars can also be used.

[0007] Especially in a market in constant growth and for ecological reasons, dispersants based on renewable raw materials are gaining more and more importance, as they allow the reduction of dependence on crude oil.

[0008] However, despite the fact that some dispersants based on renewable sources are already known and in use, it is a constant challenge to supply dispersants based on renewable raw materials that meet the requirements of cost-benefit and performance ratios.

[0009] However, renewable raw materials or by-products of industrial processes can comprise a relatively large amount of halides, especially chlorides. In particular, the chloride contents can be up to 1-10% by weight. When using such materials, for example, as dispersants or setting retardants for binder compositions, corrosion of reinforcement structures can be

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3/25 make it a serious problem. Consequently, there are standards or recommendations that regulate the maximum permitted chloride content in concrete additives (see, for example, standard EN 934-1) or in concrete (see, for example, standard EN 206-1, recommendation ACI 222R or ACI 318 / 318R). Therefore, several renewable raw materials cannot be used as a concrete additive due to its high chloride content, although the reduction of water or the retarding properties of the concrete grip are sufficient. Thus, they can only be used if they have been previously purified.

[0010] In this regard, WO 2005/062800 A2 (Batchelder et al.) Describes a process in which an industrial waste feed stream containing ligninosulfonate is treated by electrodialysis and filtration to remove solids and certain small molecules and ionizable components present in the flow, to form an improved quality lignosulfonate product. However, electrodialysis is a complicated and costly technique.

[0011] There is, therefore, a need to develop new and improved solutions that reduce or overcome the disadvantages mentioned above.

Disclosure of the invention [0012] It is an object of the present invention to provide methods and dispersants that do not have the above mentioned disadvantages. In particular, an advantageous method must be provided for the production of dispersants based on renewable raw materials or by-products of industrial processes. Preferably, the method should allow the production of dispersants with the lowest possible loss of active raw material, with a high yield and without the need for excessive maintenance, cleaning or regeneration of the equipment. At the same time, the method must make it possible to obtain dispersants with a high solids content. In particular, the method must also allow for the production of

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4/25 dispersants with a proportion of halides, especially chlorides, as low as necessary for applications such as concrete additives, particularly as low as necessary to meet local standards regarding the content of chlorides in additives or in concrete. In addition, it must be possible to obtain the most economical dispersants possible.

[0013] Surprisingly, it has been discovered that the problem of the invention can be solved according to claim 1. Thus, the main objective of the invention is to provide a method for the production of a dispersant for mineral suspensions comprising the steps of:

a) Provide a vinasse type material as an input;

b) Pass the input through at least one nanofiltration step in order to separate the input into a retentate phase and at least one filtrate phase;

c) Collect the retentate phase previously obtained and supply it as a dispersant.

[0014] As shown, the method according to the invention allows a very efficient reduction of the concentration of halides, especially of the concentration of chlorides, in vinasse-type materials that are by-products of industrial processes. In particular, the concentration of halides can be easily reduced to meet local standards with respect to the content of chlorides in additives, for example, according to EN 934-1.

[0015] In addition, the method according to the invention allows directly treating liquids of vinasse type materials with a high solids content, for example, in the range of 30% by weight or more, at very low temperatures, for example, from 25-40 ° C with very high feed rates. Thus, the loss of vinasse-type materials proved to be very low. At the same time, the inventive method does not require excessive maintenance, cleaning or needs to regenerate the nanofiltration stage. This is highly advantageous from an economic and

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5/25 ecological, since the amount of energy and time required to produce dispersants can be reduced to a minimum.

[0016] The fact that an effective reduction in the concentration of halides can be achieved in combination with a low loss of vinasse type materials and a high yield is seen with great surprise. Normally, by effectively reducing impurities in the materials to be cleaned, a large amount of the material to be cleaned is lost. However, surprisingly, this occurs to a much lesser extent with the method according to the invention.

[0017] Furthermore, it has been demonstrated that the method according to the invention can be used to increase the solids content of vinasse type materials. Thus, while reducing the proportion of halides in vinasse type materials, it is possible, at the same time, to increase the solids content of vinasse type materials. This is highly interesting, for example, in terms of transport, as a reduced amount of water will reduce the total weight and volume to be transported without reducing the total amount of active or solid material.

[0018] Furthermore, vinasse-type materials produced according to the method according to the invention have proved to be highly suitable as additives for conventional dispersants. In addition, vinasse-type materials produced in accordance with the present invention have been shown to be compatible with many conventional dispersants and other concrete additives.

[0019] Other aspects of the invention are the subject of other independent claims. Especially preferred embodiments of the invention are the subject of the dependent claims.

Ways of carrying out the invention [0020] A first aspect of the invention concerns a method for producing a dispersant for mineral suspensions comprising the steps of:

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6/25

a) Provide a vinasse type material as an input;

b) Pass the input through at least one nanofiltration step in order to separate the input into a retentate phase and at least one filtrate phase;

c) Collect the retentate phase previously obtained and supply it as a dispersant.

[0021] According to another aspect, the invention concerns the use of at least one nanofiltration stage for the production of a dispersant for mineral suspensions of vinasse type materials. Thus, the use preferably comprises the steps of:

a) Provide a vinasse type material as an input;

b) Pass the input through at least one nanofiltration step in order to separate the input into a retentate phase and at least one filtrate phase;

c) Collect the retentate phase previously obtained and supply it as a dispersant.

[0022] In particular, the nanofiltration stage is not used in combination with an electrochemical based filtration stage. In particular, the nanofiltration stage is not used in combination with an electrodialysis stage. In particular, this means that neither the input provided to the nanofiltration stage nor a retentate phase and / or a filtrate phase is passed through an electrochemistry-based filtration stage or an electrodialysis stage.

[0023] In the present context, a vinasse-type material refers, in particular, to materials comprising or consisting of by-products obtained in industrial processes involving processing and / or fermentation of sugar and / or sugar derivatives. In particular, a vinasse type material is a by-product of the production of bioethanol, yeast and / or citric acid and / or a by-product of the processing of corn and / or starch. In particular, vinasse-type materials are derived from

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7/25 sugar cane, sugar beet, corn and / or starch, especially sugar cane and / or sugar beet. In addition, the vinasse type material can, for example, be a maceration liquor. This is, as a rule, obtained as a by-product of wet corn milling. Such materials are typically fluid or liquid and comprise a certain amount of water. It is possible that these materials are also available in powder form. Preferably, the vinasse type material or the input, respectively, is a liquid.

[0024] According to a preferred modality, the vinasse type material consists of vinasse, in particular vinasse derived from sugar cane and / or sugar beet. With the method according to the invention, vinasse can be treated in an especially efficient manner.

[0025] In particular, the content of halides, especially the content of chlorides, of the vinasse-type material used in the present invention is 110% by weight, especially 2.5 - 5% by weight, in relation to dry weight of vinasse type materials.

[0026] Vinasse-type materials, obtained as by-products of industrial processes, can have a solids content of 3 to 5% by weight in relation to the total weight of vinasse-type materials. Preferably, however, vinasse-type materials are concentrated, for example, by removing or evaporating water, to obtain a higher solids content for use in the present invention.

Thus, in a particularly preferential way, the vinasse-type materials or inputs used in the present invention may initially have a solids content of about 10 - 70% by weight, especially 20 - 60% by weight or 30 - 60% by weight in relation to the total weight of the vinasse type material or the input, respectively. Depending on the feed material used in the vinasse production processes (bioethanol, citric acid or yeast), the composition of the vinasse

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8/25 may vary. Preferably, in the present context, a sugar content of vinasse can be from 0.5 to 20% by weight, especially from 2 to 15% by weight, relative to the dry weight of the vinasse. A proportion of protein can be in the range of 8 to 50% by weight, especially 10 to 40% by weight, in relation to the dry weight of the vinasse. In particular, vinasse is derived from sugar cane and / or sugar beet.

[0028] Vinasse-type materials must be purified using a filtration method. Nanofiltration is a membrane-based filtration method that uses, in particular, nanometer-sized pores that pass through the membrane. As a rule, a pore size in nanofiltration is about 0.001 - 0.002 pm, especially about 0.001 pm. A molecular weight cut (MWCO) with nanofiltration is, in particular, in the range of 100 - 8,000 Daltons. The molecular weight limit refers, in particular, to the molecular weight at which 90% of the analytes (or solutes) are prevented from crossing the membrane.

[0029] In the present context, the filtrate is the phase that predominantly crosses the membrane, while the retention phase is the phase that is retained or maintained by the membrane.

[0030] Nanofiltration should not, however, be confused with microfiltration, ultrafiltration or reverse osmosis: although microfiltration is also a membrane-based separation process, the pore size is about 0.03 to 10 pm and a molecular weight cut (MWCO) is generally greater than 100,000 Daltons. With ultrafiltration, the pore size is about 0.002 to 0.1 pm and the MWCO is about 10,000 to 100,000 Daltons. In reverse osmosis, the pore size is even smaller than with ultrafiltration, and the MWCO is less than 100 Daltons. Thus, nanofiltration membranes have smaller pore sizes than those used in microfiltration and ultrafiltration, but larger than in reverse osmosis.

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9/25 [0031] Preferably, at least one nanofiltration step comprises a membrane with a molecular weight cut (MWCO) in the range of 100 - 8,000 Daltons, especially 110-5,000 Daltons, particularly 150-1,000 Daltons, of especially preferred form of 200 - 800 Daltons, for example 200 - 300 Daltons.

[0032] When using nanofiltration technology with pore sizes or MWCO so small to separate halides from small organic materials such as organic acids, proteins, sugars etc., it would normally be expected that i) with a small pore size, only halides are separated while the yield is very low, or ii) with a larger pore size, a higher yield can be achieved, but in addition to the halides, a significant amount of small organic material also passes through the membrane and, consequently, is lost .

[0033] Surprisingly, it has now been discovered that, using this technique with vinasse type materials, an effective separation of halides is possible without high losses of active materials in combination with a high yield.

[0034] In particular, the at least one nanofiltration phase comprises an inorganic and / or organic membrane, especially an organic membrane, preferably a membrane based on polyamide and / or a membrane based on polysulfone.

[0035] Such membranes have proved to be especially advantageous when producing dispersants from vinasse type materials. In particular, these membranes allow the effective removal of halides, especially chlorides, and at the same time, obtaining a high input yield. However, for specific purposes or other inputs, other membranes with a different molecular weight cut or made from other materials can also be useful.

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10/25 [0036] According to an especially preferred modality, step b) comprises or consists of the following substeps:

b1) Pass the input through a first nanofiltration stage in order to obtain an intermediate retentate stage and a first filtrate stage and b2) Pass the intermediate retentate stage again through the first nanofiltration stage and / or a second stage of nanofiltration, in order to obtain the retentate phase and a second filtrate phase.

[0037] Thus, the first nanofiltration stage may be different from the second nanofiltration stage. For example, the membrane of the first stage of nanofiltration may be different from the membrane of the second stage of nanofiltration, for example, in terms of the cut of molecular weight, membrane material, size and / or pore structure.

[0038] The use of at least two stages of nanofiltration in series helps to surprisingly optimize the removal of halide atoms, especially chloride atoms, while ensuring a high yield of the input without clogging the membrane pores.

[0039] It is also possible to provide for additional nanofiltration steps. Thus, the retentate phase of an earlier nanofiltration stage is preferably passed through an additional nanofiltration stage. In addition, this procedure helps to reduce the proportions of halide atoms, especially chloride atoms, in the retentate or dispersant, respectively.

[0040] In another preferred embodiment, the intermediate retentate obtained in step b) is diluted with a solvent, especially with water, before passing the intermediate retentate phase again through the first nanofiltration phase and / or a second nanofiltration phase. For dilution, in relation to the total weight of the intermediate retentate obtained in step b), 5 - 50% by weight are added, in particular 10 - 30%

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11/25 by weight of solvent to the intermediate retentate. This dilution helps to further improve the overall process.

[0041] The reduction in the concentration of halides depends on the initial proportion of halides in the input and the desired level of halides in the dispersant. Thus, preferably, the parameters of the method according to the invention are adapted accordingly.

[0042] For example, if a dispersant consists of 30% by weight of vinasse and 30% by weight of vinasse has a chloride content of 0.65% by weight, the chloride content will need to be reduced by 86% to obtain a final chloride proportion of 0.09% by weight in the dispersant that is, for example, in line with the EN 934-1 standard.

[0043] In another example, if a dispersant contains only 25% of a vinasse at 30% by weight and the vinasse at 30% by weight has a chloride content of 0.65% by weight, a content four times higher of chloride vinasse at 30% by weight can be accepted. This means that the chloride content of vinasse at 30% by weight has to be reduced from 0.65% by weight to a target concentration of 0.36% by weight, which corresponds to a reduction of only 45%. The final blend based on 25% vinasse at 30% with a final chloride content of 0.36% by weight would exceed the standard EN 934-1 with a final chloride concentration of 0.09%.

[0044] In particular, a concentration of halides, in particular a concentration of chlorides, in the retentate phase collected in step c) reduced by> 10% by weight, especially by 30% by weight, particularly by> 50% by weight, preferably> 70% by weight or even> 90% by weight, in relation to the halide concentration of the vinasse type input provided in step a).

[0045] In particular, a concentration of halides, in particular a concentration of chlorides, in the retentate phase collected in step c) reduced by 10 - 100% by weight, especially by 20 - 90% by weight, particularly by 30 - 80 % by weight or 50 - 80% by weight

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12/25 regarding the concentration of halides of the vinasse type input provided in step a).

[0046] Advantageously, a concentration of organic material, for example, acids and proteins and / or salts of organic acids, in the retentate phase reduced by less than 25% by weight, especially by less than 10% by weight, particularly less 5% by weight, preferably less than 2% by weight or less than 1% by weight, in relation to the concentration of organic material in the vinasse type input.

[0047] Preferably, the solids content of vinasse-type materials or inputs is increased when performing the inventive method. In particular, the solids content of vinasse-type materials is increased by at least 5%, particularly by at least 10%, especially by at least 25%, preferably by at least 40% or at least 60%, in relation to the content of solids of vinasse type materials. Increasing the solids content is very advantageous because logistical costs can be reduced during transport.

[0048] However, the method can also be carried out without concentrating vinasse type materials.

[0049] Especially preferably, the method or use according to the invention does not comprise any electrochemically induced separation processes, in particular, it does not comprise the electrodialysis of the input and / or a retention phase. As discovered in the present context, electrochemically induced separation processes, such as electrodialysis, remove at least part of organic materials, in particular acids and acid salts, from the input. This, in turn, leads to less water reduction when using purified vinasse type materials as plasticizers for hydraulic handle compositions.

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13/25 [0050] Furthermore, the method or use according to the invention does not comprise any ion exchange processes for the input and / or a retention phase. Due to the high proportions of halides to be removed from vinasse type materials, ion exchange requires excessive maintenance, cleaning or regeneration. From an economic point of view and in terms of technical effort, such processes are disadvantageous in the present context.

[0051] However, for specific purposes, additional electrochemically induced separation processes or even purification steps using ion exchange technologies or their combinations may also be an option.

[0052] According to a preferred modality, in step b) and / or during nanofiltration, the vinasse type material is subjected to a pressure of 0.5 - 500 kg / cm ² , especially 1 - 250 kg / cm ² , particularly 5 - 100 kg / cm ² , preferably 10 - 75 kg / cm ² or 20 - 50 kg / cm ² . Here, the pressure is given in relation to a conventional standard value of the gravitational constant of 9.80665 m / s ² .

[0053] Also preferably, step b) is carried out at a temperature of 5 - 95 ° C, especially at 10 - 75 ° C, particularly at 15 - 55 ° C, particularly preferably at 20 45 ° C or from 22 - 28 ° C. In particular, the temperature during step b) is a maximum of 55 ° C, preferably a maximum of 45 ° C, especially a maximum of 40 ° C.

[0054] In particular, a feed rate for vinasse-type material in step b) is 1 - 100 m ³ / h, especially 2 - 75 m ³ / h, particularly 3 - 50 m ³ / h, particularly preferred form of 5 - 20 m ³ / h.

[0055] Such process parameters have been shown to be very beneficial in terms of process efficiency, economic aspects and

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14/25 ecological aspects. This, in particular, if the dispersants are produced from vinasse.

[0056] Additionally preferably, before step b), the input is passed through a mesh filter, especially with a mesh size of about 15 - 300 pm, preferably from 25 to 200 pm, especially preferably 30 - 70 pm. The filtrate obtained in this way can then be used as an input in step b).

[0057] Even more preferably, before step b), the input is passed through a microfiltration step, especially with a pore size of about 0.1-10 pm, preferably 1-8 pm, especially preferred 3-7 pm. The filtrate obtained in this way can then be used as an input in step b).

[0058] Advantageously, the input is first passed through a mesh filter and subsequently the input is passed through a microfiltration phase. The filtrate obtained in this way can then be used as an input in step b). Advantageous mesh filters and the microfiltration stage are described above.

[0059] A mesh filter and / or microfiltration stage helps to eliminate interfering particles from the inputs, which, in turn, further increase the efficiency of the filter in the nanofiltration stage (s). However, other pre-filtration systems can also be used or pre-filtration systems can be avoided.

[0060] Another aspect of the present invention concerns a dispersant for mineral suspensions, obtainable or obtained by a method according to the invention, as described above.

[0061] Such a dispersant can be used, for example, as a dispersing, plasticizing and / or water reducing agent for mineral suspensions and / or mineral binder compositions, in particular for hydraulic handle mineral binder compositions, especially preferential for mineral binder compositions

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15/25 cementitious. However, the dispersant can also be used as a dispersing agent for other purposes.

[0062] Thus, an additional aspect of the present invention is related to the use of a dispersant as described above as a dispersing, plasticizing and / or water reducing agent for mineral suspensions and / or mineral binder compositions, in particular for compositions of hydraulic bonded mineral binder, especially preferred for cementitious mineral binder compositions.

[0063] The dispersant is used, in relation to the mineral material, especially the mineral binder, preferably with a fraction of 0.01 to 10% by weight, especially from 0.1 to 5% by weight or from 0.5 to 2% by weight. This fraction refers especially to the solids content of the dispersant.

[0064] The dispersant according to the present invention can be used alone or in combination with one or more plasticizers. Thus, one or more plasticizers are, in particular, chemically different from the dispersant according to the present invention.

[0065] According to a preferred embodiment, the dispersant according to the invention further comprises a plasticizer, especially a plasticizer selected from the group consisting of polycarboxylates, polycarboxylate ethers, vinyl copolymers, lignosulfonates, condensates of naphtalene sulphonic-formaldehyde acid, condensates of sulphonated formaldehyde melamine. According to another preferred embodiment, the dispersant according to the invention may comprise a setting retarder, which may even have plasticizing effects. The setting retarder is, for example, derived from cellulose and / or hydrolyzed starch. In particular, the setting retarder is, for example, a glucose / corn syrup (with varying amounts of glucose, oligo and polysaccharides), glucose, gluconate, products

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16/25 hydrogenated glucose and / or waste products such as other materials such as vinasse or molasses (sugar production), as well as other types of sugar or sugar acids.

[0066] Advantageously, the plasticizer involves in particular a polycarboxylate, especially a polycarboxylate ether. In particular, the plasticizer is a comb-shaped polymer that comprises a structure to which anionic groups and / or their polyalkylene glycol salts and chains are attached. Polycarboxylate ethers are usually produced in a polymerization process or through a condensation reaction analogous to that of polymers.

[0067] Such comb polymers are also marketed by Sika Schweiz AG under the brand name ViscoCrete®.

[0068] By combining with a plasticizer, the properties of the dispersant can be optimally adapted to different requirements.

[0069] In an especially preferred embodiment, the plasticizer has a fraction in the dispersant of, for example, from 1 to 95% by weight, especially from 2 to 50% by weight, particularly from 3 to 30% by weight or from 5 to 5% 20% by weight.

[0070] In addition, the dispersant may optionally comprise one or more additives, particularly a defoamer, a dye, a preservative, another dispersant, a retarder, an accelerator, an air-forming agent, a shrink reducer, a modifier viscosity, a stabilizer, a biocide and / or a corrosion inhibitor or combinations thereof.

[0071] Another aspect of the present invention relates to a mineral suspension, particularly a mineral binder composition, comprising a dispersant as described above or a dispersant that is obtainable or obtained by an inventive method as described here.

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17/25 [0072] In the present context, the term mineral suspension refers, in particular, to a heterogeneous mixture containing solid mineral particles that are dispersed throughout a fluid phase, which is particularly a liquid, containing or consisting especially of water. A weight ratio of the liquid phase to mineral particles is preferably in the range of 0.2 to 0.8, especially 0.3 to 0.7, preferably 0.4 to 0.6.

[0073] Mineral binder means, in particular, a mineral binder that reacts in the presence of water in a hydration reaction to form solid hydrates or hydrate phases. This can be, for example, a hydraulic binder (such as cement or hydraulic lime), a latent hydraulic binder (such as slag), a pozzolanic binder (such as fly ash or natural pozzolans) or a non-hydraulic binder (plaster).

[0074] In particular, a mineral binder or a mineral binder composition can be a cement binder or a cement binder composition, meaning, in the present case, particularly a binder or a binder composition with a fraction of at least 5% in weight, especially at least 20% by weight, preferably at least 35% by weight, especially at least 65% by weight of cement clinker. According to another preferred embodiment, the binder or a binder composition is composed of at least 95% by weight of cement clinker.

[0075] In particular, a cement binder or a cement binder composition is based on a cement that is defined, for example, in standards EN 197-1 or ASTM C150 or ASTM C595. A fraction of the cement clinker in the cement binder or in a cement binder composition, taken as a whole, is preferably equivalent to at least 5% by weight, especially at

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18/25 at least 20% by weight, preferably at least 35% by weight, especially at least 65% by weight. According to another preferred embodiment, the cement binder or a cement binder composition is composed of at least 95% by weight of cement clinker.

[0076] However, it may also be advantageous that the mineral binder or mineral binder composition contains other binders in addition to or instead of a hydraulic binder. These are, in particular, latent hydraulic binders and / or pozzolanic binders. Latent hydraulic binders and / or suitable pozzolanic binders are, for example, slag, fly ash, silica powder and / or natural pozzolans. Likewise, the binder composition may contain inert substances such as ground limestone, ground quartz and / or pigments. In a preferred embodiment, the mineral binder contains from 5 to 95% by weight, especially from 5 to 65% by weight, particularly from 15 to 35% by weight of latent and / or pozzolanic hydraulic binders.

[0077] In particular, the mineral suspension is a mineral binder composition containing a mineral binder and a dispersant as described above. A fraction of the dispersant in relation to the mineral binder, in particular, is 0.01 to 10% by weight, preferably 0.1 to 5% by weight or 0.5 to 2% by weight. This fraction refers especially to the solids content of the dispersant. The mineral binder and dispersant are defined here as described above. A binder composition can be present, for example, in dry form or as a fluid or hardened binder composition prepared with the addition of water.

[0078] In another preferred embodiment, the binder composition additionally contains solid aggregates, especially gravel, sand and / or aggregates. Corresponding compositions can be

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19/25 used, for example, as mortar mixes or concrete mixes.

[0079] In particular, the binder composition additionally contains water, in which a weight ratio of water to mineral binder is preferably in the range of 0.25 to 0.8, especially 0.3 to 0 , 7, preferably from 0.4 to 0.6. Such binder compositions can be processed directly as mortar mixtures or concrete mixtures.

[0080] In addition, the invention also relates to a molded body, which can be obtained by hardening a binder composition as described above after adding water. The molded body produced in this way can have almost any desired shape and can be, for example, part of a construction project, such as a building, a wall or a bridge.

[0081] Another aspect concerns a method for preparing a mineral suspension, particularly a mineral binder composition, in which a dispersant as described above is added to a mineral material, especially a mineral binder, preferably a hydraulic mineral binder. The dispersant can, for example, be mixed with the water added to the binder composition, which is then used to agitate the binder composition. It is also possible to add dispersant or the composition containing it directly to the mineral or binder material and mix it in the added water before and / or afterwards, if necessary. It is also possible that only a part of the dispersant is mixed with the added water and the other part is added before, during and / or after adding the water to the binder composition.

[0082] In addition, in a further aspect of the invention, the dispersion materials of the invention can still be added during cement production, alone or in combination with

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20/25 commercially available cement, to influence the cementability and / or the cementation properties of ground cement.

[0083] Other advantageous embodiments and combinations of features of the invention will emerge from the exemplary embodiments below and from the entirety of the patent claims. Exemplary modalities

1. Production of dispersants 1.1 Method [0084] Fig. 1 shows a schematic illustration of an inventive method for the production of dispersants.

[0085] Specifically, two different processes were executed, P1 and P2, with different sets of parameters (cf. table 1).

[0086] In both processes, the same untreated vinasse obtained from the production of bioethanol using sugar beet in sugar cane as an FM type vinasse input was used. Then, in the first stage, the FM input was passed through a MeF mesh filter and a MiF microfilter. The filtrate obtained in this way was then subjected to a two-stage nanofiltration treatment.

[0087] Thus, the pre-filtered input was passed through a first stage of nanofiltration S1, in order to obtain an intermediate retentate phase IR and a first phase of filtrate F1. Subsequently, the intermediate retentate phase IR was diluted by adding water W (20% by weight in relation to the total weight of IR) and passed through a second nanofiltration stage S2, in order to obtain the retentate phase R and a second phase of filtrate F2. Thus, the first and second stages of nanofiltration were identical in terms of membranes.

[0088] Table 1 presents an overview of the parameters used in processes P1 and P2: Table 1: Process parameters

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Parameter P1 P2 Solid content 28% by weight 28% by weight Feed rate 10 m ³ / h 10 m ³ / h Mesh filter (pore size) 50 pm 50 pm Microfilter (pore size) 5 μΜ 5 μΜ Operating pressure 28 kg / cm ² 35 kg / cm ² Temperature 25 - 40 ° C 25 - 30 ° C Nanofiltration - MWCO Membrane type N ^Q stages 250 Da Polyamide 2 720 Da Polyethersulfone (FOOT) 2

[0089] To investigate the processes, the contents of solids and the proportions of chloride ions were measured in several phases. The solids content was measured after drying at 120 ° C and the chloride content was measured according to EN 480-10. Table 2 provides an overview of the results obtained.

Table 2: Results (all figures in% by weight)

Phase P1 P2 Solids ¹⁾ Cl ² > Solids ¹⁾ Cl ²⁾ FM 27.95 2.33 27.95 2.33 GO 39.69 1.13 22.09 1.41 F1 - - 5.74 9.18 R 36.36 0.49 22.98 1.33 F2 6.62 ³⁾ 8.25 ³⁾ 3.81 8.85

1) Regarding the weight of the solids content of the respective phase

2) Regarding the solids content

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3) Content of the intermixed filtrates F1 and F2 [0090] As can be deduced from table 2, the method according to the invention allows to clearly reduce the chloride content to values below 0.5% by weight (P1) or 1.4% by weight (P2) in the final retentate phase R compared to the initial content in the FM input. Consequently, the chloride content in the filtrate phases F1 and F2 is increased significantly.

[0091] It is worth mentioning that the process conditions can be adjusted to achieve a higher solids content after the filtration process. For example, for the P1 process with vinasse obtained from the production of bioethanol, the solids content in the retentate phases (IR, R) is even higher than the solids content of the input (FM). This means that the vinasse is concentrated during the filtration process.

[0092] In this way, the method according to the invention can be used to reduce the amount of halides in vinasse type materials and, at the same time, increase the solids content of vinasse type materials.

[0093] In another test, a vinasse-type material obtained from the production of yeast was used, as disclosed in patent EP 3 026 032 A1.

[0094] When using a process parameter analogous to that of P1 (table 1) in another process P3, a reduction of chlorides similar to that of vinasse based on bioethanol can be obtained (see table 3).

Table 3: Results (all figures in% by weight)

Phase P3 Solids ¹⁾ Cl ²⁾ FM 39.14 1.49 GO 25.99 0.75

1.2 Dispersants

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23/25 [0095] The retend phase R resulting from process P2 was used as dispersant D for further tests.

[0096] Specifically, the following dispersants DO, D1 and D2 were supplied or produced, respectively:

DO: Sika® Plastocrete (a commercially available mid-range water reducing additive from Sika with a concentration of 32% by weight of lignosulfonate; for comparison).

D1: An aqueous mixture with 24% by weight of lignosulfonate and 8% by weight of dispersant D.

D2: An aqueous mixture with 16% by weight of lignosulfonate and 16% by weight of dispersant D.

2. Concrete tests

2.1 Concrete compositions [0097] The dispersants were tested in concrete mixtures. For this, a concrete with the composition specified in table 4 was used.

Table 4: Concrete mixes

Component Quantity [kg / m3] Cement (OPC type 1) 210 Fly ash 90 Aggregates 1,080 Sand 780 Water 170 liters

[0098] The dispersants were used as an aqueous solution with a fraction of 0.5% by weight of the total binder content consisting of cement and fly ash. The dispersants were mixed in advance with the amount of water used for the concrete, so that a homogeneous solution was obtained. For the production of concrete, sands, aggregates, cement and fly ash

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24/25 were added in a drum mixer and the dry mixture was mixed for 30 seconds. Then, water, including the dispersant, was added and the wet mixture was mixed for an additional 3 minutes.

2.3 Test methods [0099] In order to determine the effectiveness of the dispersant according to the invention, the slump of the concrete mixtures was measured immediately after the preparation of the concrete and also after 30 minutes and 60 minutes. In addition, the compressive strength of concrete mixtures was determined for 3 days (3 d), 7 days (7 d), 14 days (14 d) and 28 days (28 d). In addition, the setting time of the concrete mixtures was determined.

[00100] Concrete slump, compressive strength and setting times were determined according to ASTM standards.

2.4. Results [00101] Table 5 presents a summary of the results obtained with various dispersants. Please note that the D0 dispersant tests (not produced according to the invention) were made for comparison purposes.

Table 5: Effects of dispersants in concrete mixtures

Dispersant D0 D1 D2 Loss of dejection [cm] 0 min 14.0 14.0 14.0 30 min 7.0 6.0 7.0 60 min 5.5 5.0 5.0 Compressive strength after 3 days [kg / cm ² ] 262.7 246.3 255.4 Compressive strength after 7 days [kg / cm ² ] 301.2 304.9 310.3

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Compressive strength after 14 days [kg / cm ² ] 353.8 356.4 362.8 Compressive strength after 28 days [kg / cm ² ] 415.7 414.9 423.5 Pick-up time [h: min] Hardening 5:45 5:36 05:29 Initial 7:10 6:53 06:47 Final 8:40 08:15 08:08

[00102] As can be deduced from Table 5, dispersants D1 and D2, both comprising vinasse which were treated according to the method of the invention, are very similar to the commercially available DO lignosulfonate dispersant in terms of plasticizing effect , delay in grip and resistance to compression.

[00103] Thus, the data presented above clearly show that the dispersants that are produced according to the present invention have, after the purification process, the desired properties of fresh and hardened concrete. In addition, the dispersants according to the invention are compatible with existing mid-range water reducers and can be used in different combinations for this type of water reducer.

[00104] It will be appreciated by those skilled in the art that the present invention can be configured in other specific ways without departing from its spirit or its essential characteristics. Therefore, the modalities disclosed here are considered, in all aspects, as illustrative and not restrictive.

Claims (19)

1. Method for producing a dispersant for mineral suspensions, characterized by the fact that it comprises or consists of the steps of: a) Supply of vinasse-type material as an input; b) Pass the input through at least one nanofiltration step in order to separate the input into a retentate phase and at least one filtrate phase; c) Collect the retentate phase previously obtained and supply it as a dispersant. 2. Method according to claim 1, characterized by the fact that at least one nanofiltration step comprises a membrane with a molecular weight cut (MWCO) in the range of 100-8,000 Daltons, especially 110-5,000 Daltons, particularly 150-1,000 Daltons, especially preferably 200 - 800 Daltons, for example, 200 - 300 Daltons. Method according to at least any one of claims 1 - 2, characterized in that the at least one nanofiltration step comprises an organic membrane, especially a polyamide-based membrane and / or a polyethersulfone-based membrane (FOOT). 4. Method according to at least any one of claims 1 - 3, characterized by the fact that step b) comprises the steps of: b1) Pass the input through a first nanofiltration stage in order to obtain an intermediate retentate stage and a first filtrate stage and b2) Pass the intermediate retentate stage again through the first nanofiltration stage and / or a second stage Petition 870190046339, of 5/17/2019, p. 34/39 2/4 nanofiltration, in order to obtain the retentate phase and a second filtrate phase. 5. Method according to at least any one of claims 1 - 4, characterized by the fact that, before step b), the input is passed through a microfiltration step, especially with a pore size of about 0, 1-10 pm, preferably 1-8 pm, especially preferably 3-7 pm and / or where, before step b), the input is passed through a mesh filter, especially with a mesh size of about 15 - 300 pm, preferably 25-200 pm, especially preferably 30 - 70 pm. 6. Method according to at least any one of claims 1 - 5, characterized in that the method does not comprise electrochemically induced separation processes, in particular, it does not comprise electrodialysis of the input and / or a retentate phase. 7. Method according to at least any one of claims 1 - 6, characterized by the fact that a concentration of halides, in particular a concentration of chlorides, in the retentate phase collected in step c) is reduced by> 10% by weight, especially by 30% by weight, particularly by> 50% by weight, preferably by> 70% by weight or by> 90% by weight, based on the halide concentration of the vinasse type input. 8. Method according to at least any one of claims 1 - 7, characterized by the fact that a concentration of organic materials, especially organic acids and proteins and / or salts of organic acids, in the retentate phase is reduced by less than 25%, especially less than 10%, particularly less than 5%, preferably less than 2% or less than 1%, in relation to the concentration of organic material in the vinasse type input. Petition 870190046339, of 5/17/2019, p. 35/39 3/4 9. Method according to at least any one of claims 1 - 8, characterized by the fact that, in step b) and / or during nanofiltration, the vinasse type material is subjected to a pressure of 0.5 - 500 kg / cm ² , especially 1 - 250 kg / cm ² , particularly 5 - 100 kg / cm ² , preferably 10 - 75 kg / cm ² or 20 - 50 kg / cm ² . 10. Method according to at least any of claims 1-9, characterized by the fact that the solids content of vinasse-type materials or inputs is increased when the method according to the invention is carried out, by means of whereas, preferably, the solids content of vinasse-type materials is increased by at least 5%, particularly by at least 10%, especially by at least 25%, preferably by at least 40% or at least 60% in relation to solids content of vinasse type materials as provided in step a). 11. Method for producing a mineral suspension, particularly a mineral binder composition, characterized in that a dispersant obtainable or obtained by a method in accordance with at least any one of claims 1-10, is added to a mineral material, especially to a mineral binder, preferably to a hydraulic mineral binder. 12. Dispersant for mineral suspensions, characterized by the fact that it can be obtained using a method according to any one of claims 1-10. 13. Dispersant according to claim 12, characterized by the fact that it additionally comprises a plasticizer, especially a plasticizer selected from the group consisting of polycarboxylates, polycarboxylate ethers, vinyl copolymers, lignosulfonates, condensates of naphthalene sulfonic-formaldehyde acid , carbohydrates and / or condensates of sulphonated formaldehyde melamine. Petition 870190046339, of 5/17/2019, p. 36/39 4/4 14. Mineral suspension, particularly a mineral binder composition, characterized by the fact that it comprises a dispersant according to any one of claims 12 - 13 and a mineral material, especially a mineral binder. 15. Molded body, characterized by the fact that it can be obtained by hardening a mineral binder composition according to claim 14, after adding water. 16. Use of a dispersant according to at least any one of claims 12-13 or a dispersant that can be obtained using a method in accordance with at least any one of claims 1-10, characterized by the fact that it is like dispersing, plasticizing and / or water reducing agent for mineral suspensions and / or mineral binder compositions, particularly for hydraulic binder mineral binder compositions, particularly preferably for cementitious mineral binder compositions. 17. Use according to claim 16, characterized by the fact that the dispersant is obtainable or obtained using a method that does not comprise electrochemically induced separation processes, and particularly does not comprise electrodialysis of the input and / or a retentive. 18. Use of at least one nanofiltration stage, characterized by the fact that it is to produce a dispersant for mineral suspensions from vinasse type material. 19. Use according to claim 18, characterized by the fact that the nanofiltration stage is not used in combination with an electrochemical based filtration stage. In particular, the nanofiltration stage is not used in combination with an electrodialysis stage.