BE1024705B1 - Process for the preparation of solid lactic acid and lactic acid compositions thus obtained - Google Patents

Abstract

A one-step process for preparing solid lactic acid deposited on calcium lactate support which comprises (i) directly contacting lactic acid in concentrated solution with calcium carbonate, the amount of lactic acid being in excess of the amount stoichiometrically required to effect the reaction; (ii) recovering the solid lactic acid obtained on a solid support of calcium lactate and (iii) sieving the solid particles obtained. The product obtained according to the process is also described.

Description

economy

FPS Economy, SMEs, Middle Classes & Energy Intellectual Property Office

Date of issue: 06/06/2018

PATENT

Priority date:

International classification: C07C 51/41, C07C 51/43, C07C 59/08 Filing number: BE2016 / 5748 Filing date: 07/10/2016

Holder:

GALACTIC S.A.

7760, ESCANAFFLES Belgium

Inventor:

MORLOT Julien 7760 ESCANAFFLES Belgium

COSZACH Philippe 7760 ESCANAFFLES Belgium

Process for the preparation of solid lactic acid and lactic acid compositions thus obtained

We describe a one-step process for preparing solid lactic acid deposited on a calcium lactate support which consists in (i) bringing the lactic acid in concentrated solution with calcium carbonate into direct contact, the quantity of the lactic acid being in excess relative to the stoichiometric amount necessary to carry out the reaction; (ii) recovering the solid lactic acid obtained deposited on a solid support of calcium lactate and (iii) sieving the solid particles obtained. The product obtained according to the process is also described.

BELGIAN INVENTION PATENT

FPS Economy, SMEs, Middle Classes & Energy

Publication number: 1024705 Deposit number: BE2016 / 5748

Intellectual Property Office International Classification: C07C 51/41 C07C 51/43 C07C 59/08 Date of issue: 06/06/2018

The Minister of the Economy,

Having regard to the Paris Convention of March 20, 1883 for the Protection of Industrial Property;

Considering the law of March 28, 1984 on patents for invention, article 22, for patent applications introduced before September 22, 2014;

Given Title 1 “Patents for invention” of Book XI of the Code of Economic Law, article XI.24, for patent applications introduced from September 22, 2014;

Having regard to the Royal Decree of 2 December 1986 relating to the request, the issue and the maintenance in force of invention patents, article 28;

Given the patent application received by the Intellectual Property Office on 07/10/2016.

Whereas for patent applications falling within the scope of Title 1, Book XI of the Code of Economic Law (hereinafter CDE), in accordance with article XI. 19, §4, paragraph 2, of the CDE, if the patent application has been the subject of a search report mentioning a lack of unity of invention within the meaning of the §ler of article XI.19 cited above and in the event that the applicant does not limit or file a divisional application in accordance with the results of the search report, the granted patent will be limited to the claims for which the search report has been drawn up.

Stopped :

First article. - It is issued to

GALACTIC S.A., Place d'Escanaffles 23, 7760 ESCANAFFLES Belgium;

represented by

PRONOVEM - Office Van Malderen, Avenue Josse Goffin 158, 1082, BRUXELLES;

a Belgian invention patent of 20 years duration, subject to payment of the annual fees referred to in article XI.48, §1 of the Code of Economic Law, for: Process for the preparation of solid lactic acid compositions and lactic acid thus obtained.

INVENTOR (S):

MORLOT Julien, GALACTIC S.A. Place d'Escanaffles 23, 7760, ESCANAFFLES;

COSZACH Philippe, GALACTIC S.A. Place d'Escanaffles 23, 7760, ESCANAFFLES;

PRIORITY (S):

DIVISION:

divided from the basic application: filing date of the basic application:

Article 2. - This patent is granted without prior examination of the patentability of the invention, without guarantee of the merit of the invention or of the accuracy of the description thereof and at the risk and peril of the applicant (s) ( s).

Brussels, 06/06/2018, By special delegation:

BE2016 / 5748

Process for the preparation of solid lactic acid and lactic acid compositions thus obtained

Field of the invention

The present invention relates to a process for the preparation of lactic acid compositions in solid form, in particular deposited on a support.

In particular, the method of the present invention relates to a method comprising fewer steps than the usual methods in the matter.

More specifically, the method of the invention makes it possible inter alia to combine the step of preparing calcium lactate involved in the final composition with the step of dispersing lactic acid.

The present invention also relates to the solid lactic acid thus obtained according to the process of the invention.

Lactic acid is generally obtained in the form of a syrupy liquid, which is difficult to handle; this is why for its use it is put in the form of an aqueous solution, or else it is put in the form of small solid particles mixed with or deposited on a support which is most often calcium lactate.

In both cases, whether in the form of an aqueous solution or in the form of solid particles, the usual methods include numerous operations in order to obtain a lactic acid which is easy to handle and easily usable in compositions used in the food sector or more especially. in the bakery and confectionery sector.

At present, the usual methods for obtaining solid particles of lactic acid comprise several complex steps which require substantial investment.

BE2016 / 5748

To this end, mention may in particular be made of (i) the preparation of an aqueous solution of calcium lactate (at around 30% by weight) by reaction of lactic acid and whitewash and (ii) spraydrying (drying by spraying) of this aqueous solution to obtain solid calcium lactate pentahydrate; then, (iii) this calcium lactate must be dried in a fluidized bed in order to obtain anhydrous calcium lactate, which will serve as a support on which we just (iv) disperse lactic acid which we can (v) dry depending on the desired water concentration.

It is therefore easy to see that this process is long and tedious and that it requires substantial investment.

There is therefore a need for a simple and less expensive method for obtaining solid lactic acid on a calcium lactate support.

The object of the present invention is a simple process for obtaining solid lactic acid dispersed on a calcium lactate support.

Another objective is a process which comprises only one step for preparing support and supported lactic acid.

Another objective is to considerably reduce the duration of the operations which constitute the process.

Another objective of the invention is solid lactic acid on a calcium lactate support obtained according to the process of the invention and which can be in the form of a powder containing 45 to 70% by weight of lactic acid, 29.5 to 54.5% by weight of calcium lactate and 0.5 to 3% by weight of water.

The Applicant has now found a new one-step process for preparing solid lactic acid deposited on a calcium lactate support which consists in (i) bringing lactic acid into direct contact in concentrated solution with calcium carbonate , the quantity of lactic acid being in excess compared to the quantity stoichiometrically necessary to carry out the

BE2016 / 5748 reaction; (ii) recovering the solid lactic acid deposited on a solid support of calcium lactate.

According to the process of the present invention, a concentrated solution, between 90 and 99.5% lactic acid, is brought into contact with calcium carbonate. For this purpose, it is possible to start with a commercial lactic acid which will have been subjected to evaporation to obtain the concentration required for the process of the invention. Although a concentration of 90% is already sufficient, it is preferable to start from a concentration between 94 and 99.5%. This initial mixture contains an amount of lactic acid in excess of the amount stoichiometrically necessary for the reaction.

This initial mixture is relatively fluid.

CaCO3 is allowed to react with lactic acid for about 5 to 30 minutes depending on the concentration of the acid.

This step being exothermic, care will be taken to maintain the product at a temperature below 80 ° C, or even below 60 ° C.

This reaction is carried out in a reactor fitted with a stirring system capable of operating at high viscosities, for example of the order of 10,000 to 100,000 centipoise (cps).

During the reaction time, the reaction mixture passes from the fluid to viscous or even pasty state before finally reaching its solid form which is constituted by solid lactic acid on a calcium lactate support.

The carbon dioxide formed during the reaction is removed in gaseous form.

According to the process of the invention, the excess lactic acid is thus deposited on the support of calcium lactate formed during the reaction, which is a considerable advantage over the previous processes.

According to the process of the present invention it is preferable that the ratio between the amount of lactic acid and the stoichiometrically necessary amount is within a range between 2 and 4, preferably between 2.5 and 3 in order to obtain a product

BE2016 / 5748 conforms to the specifications currently desired by the market, without this being a limitation. The final product thus obtained, consisting of solid lactic acid on a calcium lactate support generally comprises from 53 to 62% by weight of lactic acid, from 37 to 44% by weight of calcium lactate and of the order of 0 , 5 to 3% by weight of water, the sum of these three constituents forming 100%.

Depending on the initial concentration of lactic acid, the product is then subjected to a drying operation, for example in a fluidized bed in dry air at a temperature between 20 and 80 ° C, ideally between 40 and 65 ° C to remove residual moisture; the solid particles of lactic acid deposited on the support are then recovered and subjected to sieving.

If the particle size of the particles thus recovered and sieved is not satisfactory for its use in market applications, these particles can be subjected beforehand to adequate grinding to obtain a powder.

If the flowability is not satisfactory, an anti-caking agent such as for example silica or magnesium stearate can be added to the sieved powder in proportions which can vary from 0.05 to 3%.

According to the process of the invention, gluconic acid can also be used in place of lactic acid.

The process of the present invention is also described with the aid of the examples below which in no way constitute a limitation.

Example

Was mixed in a High Shear Mixer type reactor, equipped with a stirring system for high viscosities, an aqueous solution of lactic acid concentrated to 99.2% by weight, with an amount of CaCO3 such that the ratio between the amount of lactic acid and the

BE2016 / 5748 stoichiometrically necessary quantity is 2.9, or if this weight ratio is expressed we will have 2054g of lactic acid solution for 392g of CaCO3.

The reaction between these two components lasted 20 minutes and during this time the temperature was maintained at a temperature less than or equal to 65 ° C by cooling the walls of the reactor.

CaCO3 thus reacts with lactic acid to form calcium lactate and excess lactic acid is deposited on the support of calcium lactate thus formed.

During the reaction, the viscosity of the reaction mixture was 65,000 cps.

At the end of the reaction, the mixture has become very pasty and finally solid and is in the form of a heterogeneous powder (small blocks, beads and powder). This powder was screened at 5 mm and subjected to drying in a fluidized bed under dry air maintained at a temperature of 52 ° C.

Finally, the solid particles of solid lactic acid on a completely dry calcium lactate support were recovered at the bottom of the fluidized bed.

These solid particles were sieved to obtain a regular particle size.

The characteristics of the product screened at <710 µm are described below.

For the record, the percentages are expressed by weight.

Lactic acid 59.9% Calcium lactate 39.1% Water 1.0% pH (10% solution) 3.1

BE2016 / 5748

Claims (11)

Claims 1. A single-step process for preparing solid lactic acid deposited on a calcium lactate support, characterized in that it consists of (i) bringing lactic acid into direct contact in concentrated solution with calcium carbonate , the amount of lactic acid being in excess relative to the amount stoichiometrically necessary to carry out the reaction; (ii) recovering the solid lactic acid obtained deposited on a solid support of calcium lactate and (iii) sieving the solid particles obtained. 2. Method according to claim 1, characterized in that the solid particles of calcium lactate deposited on the support are ground in order to obtain a powder of desired particle size. 3. Method according to claim 1, characterized in that the starting lactic acid solution is an aqueous solution whose concentration is between 90 and 99.5% by weight. 4. Method according to claim 2 characterized in that the concentration of the starting lactic acid solution is preferably between 94 and 99.5% by weight. 5. Method according to any one of claims 1 to 4, characterized in that the reaction (i) is carried out with a ratio between the amount of lactic acid and the amount stoichiometrically necessary for carrying out this reaction comprised between 2 and 4 and preferably between 2.5 and 3. 6. Method according to any one of claims 1 to 4 characterized in that one controls the temperature of the reaction (i) so that it remains below 80 ° C and 2016/5748 BE2016 / 5748 preferably below 60 ° C with adequate stirring to treat viscosities between 10,000 and 100,000 cps. 7. Solid lactic acid on a calcium lactate support obtained according to the process claimed according to any one of Claims 1 to 6. 8. Solid lactic acid on calcium lactate support according to claim 7 characterized in that it contains from 58 to 10 62% by weight of lactic acid, from 37 to 41% by weight of calcium lactate and from 0.5 to 3% by weight of water, the sum of these three constituents forming 100% by weight. 9. Solid lactic acid on calcium lactate support according to 15 claim 7 characterized in that it contains from 53 to 57% by weight of lactic acid, from 40 to 44% by weight of calcium lactate and from 0.5 to 3% by weight of water, the sum of these three constituents forming 100% by weight. 2016/5748 BE2016 / 5748 SHORT Process for the preparation of solid lactic acid and lactic acid compositions thus obtained A single-step process for preparing solid lactic acid deposited on a calcium lactate support is described which consists of (i) bringing the lactic acid in concentrated solution with calcium carbonate into direct contact, the quantity 10 of lactic acid being in excess relative to the stoichiometric amount necessary to carry out the reaction; (ii) recovering the solid lactic acid obtained deposited on a solid support of calcium lactate and (iii) sieving the solid particles obtained. The product obtained according to the process is also described. SAMENWEOKWGSVERDRAQ INZÄJCE ÖCTRÖCMEN