De methode voor de voorbereiding van de choline chloride poeders van deze uitvinding

This invention is concerned with a powdered form of Cholinechloride which has a higher Cholinechloride content than hitherto known with retention of desirable flow and storage properties, en een werkwijze voor dit product.

Choline chloride is chemisch (2-hydroxyethyl)trimethylammoniumchloride. It is a source of choline which is one of the vitamin B-complex. It finds commercial use as a nutritional factor, primarily as a dietary supplement for poultry and swine, and for pharmaceutical applications. The compound in the pure, anhydrous state is a white, crystalline solid which is very soluble in water or alcohol. It is quite hygroscopic and very rapidly picks up enough moisture to become a syrupy liquid. Bijgevolg, choline chloride is usually sold as a water solution-a 70% concentration is a common commercial form.

Cholinechloride – DIETARY REQUIREMENTS OF BROILERS

Choline supplementation in broilers shows a linear response in weight gain up to 1115mg/kg from 10-22 dagen oud. Increasing choline content up to 2000mg/kg further increases the weight gain but over and above this value no significant increase in weight gain was observed. Thus it could be concluded that excess level of choline supplementation had no additional benefit.

Cholinechloride – DIETARY REQUIREMENTS OF LAYERS

Lagen, like broilers, have an essential requirement for choline. Choline is required for the formation of a phospholipid lecithin, a component of egg yolk. Current NRC recommendations for choline allowances in laying hens are 105 mg/day for white egg layers and 115 mg/day for those laying brown eggs. On an average for the two groups it can be concluded that required dietary concentration of choline at feed intake levels of 100 en 110 g/day respectively, is approximately 1100 mg/kg.
There are several factors which influence a hen’s requirement for choline, like age, feed intake and dietary crude protein or methionine levels. It is generally accepted that dietary requirement declines with age, possibly associated with an increasing feed intake. Methionine is the first limiting amino acid for egg production and, given the common function with choline in methyl group donation, interactions between the two nutrients may be anticipated. Choline requirement in layers also varies according to the methionine and cysteine levels in feed. A diet rich in M+C has low requirement of choline and vice-versa.

The following examples illustrate the method of preparation for the choline chloride powders of this invention.

Voorbeeld 1 Preparations using Diluex clay (een) Spray drogen van een waterige slurry van choline chloride en diluex.

Een slurry werd bereid door te mengen 970 pond van een 63% waterige choline chloride -oplossing en 300 pond diluex klei. Deze slurry werd verhit 140 F. en had een viscositeit van 480 centipoises. De slurry werd gepompt naar een spuitdroger van een diameter van 10 voet en bij een druk van een druk van 1500 pond per vierkante inch door middel van een mondstuk in de droger. Het slurry, Na pompen, bleek in dezelfde tijd te zijn. Op deze manier, Een aanzienlijk uniform oppervlak -impregnatie van de gedroogde choline -chloride -deeltjes trad op. Het vaste product werd gescheiden door middel van een cyclooncollector en ontladen in een container. De volgende tabel geeft details over deze voorbereidingen, die allemaal een stal gaven, Droog, vrij stromen Choline Chloride poeder Geschikt voor commercieel gebruik.

TABLE.-POWDER-ED CHOLINE CHLORIDE PREPARATIONS Introducted Into Spray Dryer Product Length Of Solids Example Choline Additive Run (min) Recovered, Choline Chloride Percent Chloride, water, (droge basis) Percent Percent lbs. Kind Lbs.

12 Diluex clay 8.3 62 86 58 2.6 13. 7 (1de 4. 2 62 100 68 2. 2 18 do 5. 2 68 90 78 1.9 19 Attaclay X250. 4. 5 73 94 80 1. 1 11 Barden clay 1. 4 45 100 85 1. 6 20 Walnut shell flour 3. 5 75 94 78 1.2 14 Dilllex clay+Cab-O-Sil at 9:1 4 59 97 74 2′ 1 wt. verhouding. 22 Diluex clay+Oab-O-Sil at 5. 6 100 99 75 2. 3

97.5125 wt. verhouding. 19 Diluex clayd-Sodium bicarbon- 4 95 96 76 2.3

ate at 9:1 wt. verhouding.

periodically blocked the flow of the product into the collecting drums and necessitated hammering on the walls to again start the flow. The dried choline chloride powder caked in the collecting drums. The amount of solid recovered from the collector represented 64% van de 912 lbs. theoretical. By cleaning out the dryer, another 15% of the solid product was recovered, thus increasing the total solids accountability to 79%. The product was found by analysis to contain 65% Cholinechloride.

By this method, there was ditficulty with the viscosity of the original slurry increasing, with solids adhering to the walls of the drying and collecting system, with caking of the product, and with poor yields.

(B) Spray drying by separate feeding of aqueous choline chloride solution and Diluex.

Another preparation was made in the same spray dryer and with the same drying conditions except that the choline chloride solution was atomized alone while the Diluex clay was fed directly into the top of the dryer. The clay was supplied at such a rate that approximately 1 lb. of it was fed into the dryer for every 3.2 lbs. of the choline chloride solution which was atomized. The solids on the walls of the dryer rapidly reached an equilibrium depth and flowed readily through the collecting system. Er werd geen problemen ervaren bij het ontladen van de vaste stoffen van de cycloon -collector. Het product stroomde vrij in de containertrommels en cake niet. De vaste stof die in de drums was verzameld, bedroeg 82% van de vaste stoffen die in de droger worden gevoed en een gedeeltelijke reiniging van de droger verhoogde deze hoeveelheid tot 87%. Het resulterende droog, vrij stromende vaste stof die door analyse is opgenomen 72% Cholinechloride.

Andere voorbeelden Een reeks runs werd gemaakt op een manier van die beschreven in voorbeeld 1(B), Maar met behulp van een spuitdroger van 4 voet diameter. Lucht werd doorgegeven met het tempo van 250 kubieke voet per minuut en kwam de kamer binnen bij een temperatuur van ongeveer 170 naar 210 C. en liet het achter bij een temperatuur van ongeveer 110 C. een 63% waterige oplossing van cholinechloride werd geassemiseerd in de kamer van de spuitdroger door een mondstuk bij een druk van 100 pond per vierkante inch. The powdered additive was introduced into the top of the drying chamber near the air inlet by means of a screw-type conveyor. The rate of introduction of the two feed streams into the drying chamber was adjusted so that both materials were added in approxi- In the same manner, other aqueous choline chloride solutions up to concentration may be used and the amount of the powdered additive may be varied so that the final product contains choline chloride up to The choline chloride powders of this invention may be used alone or in admixture with other materials commonly used in animal feeds. Likewise, the powder may be shaped into other forms, such as pellets, if desired.

By means of this invention, there are provided new choline chloride powders of high choline chloride content which are essentially dry, free-flowing and stable, and which are made by a novel and economic process. Such a product fulfills a long standing commercial need.

We claim:

1. A stable, substantially dry, free-flowing powder comprising choline chloride substantially encapsulated by a powdered additive selected from the group consisting of attapulgite clay, a mixture of attapulgite clay and a second additive selected from the group consisting of silica gel and sodium bicarbonate wherein said second additive is no more than 10% of the Weight of the mixture, kaolinite clay, a mixture of kaolinite clay and a second additive selected from the group consisting of silica gel and sodium bicarbonate wherein said second additive is no more than 10% of the weight of the mixture, walnut shell flour, and a mixture of walnut shell flour and a second additive selected from the group consisting of silica gel and sodium bicarbonate wherein said second additive is no more than 10% of the Weight of the mixture, said powder containing 68% naar 85% choline chloride on an anhydrous weight basis.

2. A stable, substantially dry, free-flowing powder comprising choline chloride substantially encapsulated by an attapulgite clay, said powder containing from about 68% to about 85% of choline chloride on an anhydrous weight basis.

3. A stable, substantially dry, free-flowing powder comprising choline chloride substantially encapsulated by an attapulgite clay having an average particle size of 1.6 naar 1.9 microns, said powder containing from about 68% to about 85% of choline chloride on an anhydrous weight basis.

4. A stable, substantially dry, free-flowing powder comprising choline chloride substantially encapsulated by a mixture of an attapulgite clay and sodium bicarbonate wherein the sodium bicarbonate is no more than 10% of the mixture, said powder containing from about 68% to about 85% of choline chloride on an anhydrous weight basis.

5. A stable, substantially dry, free-flowing powder comprising choline chloride substantially encapsulated by a kaolinite clay, said powder containing from about 68% to about 85% of choline chloride on an anhydrous weight bas s.

6. A stable, substantially dry, free-flowing powder comprising choline chloride substantially encapsulated by walnut shell flour, said powder containing from about 68% to about 85% of choline chloride on an anhydrous weight basis.

7. In a spray-drying process for the production of a v stable, substantially dry, free-fiowing powder containing from 68% to about 85% by weight of choline chloride substantially encapsulated by a powdered additive selected from the group consisting of attapulgite clay, a mixture of attapulgite clay and a second additive selected from the group consisting of silica geland sodium bicarbonate wherein said second additive is no more than 10% of the weight of the mixture, kaolinite clay, a mixture of kaolinite clay and a second additive selected from the group consisting of silica gel and sodium bicarbonate wherein said second additive is no more than 10% of the Weight of the mixture, walnut shell flour, and a mixture of walnut shell flour and a second additive selected from the group consisting of silica gel and sodium bicarbonate whereinsaid second additive is no more than 10% of the weight of the mixture, the steps comprising (een) atomizing an aqueous choline chloride solution into the drying chamber of a spray dryer,

(B) simultaneously feeding into the drying chamber as a separate feed said powdered additive, en.

(C) collecting the choline chloride powder which has become impregnated with the powdered additive.

8. In a spray-drying process for the production of a stable, substantially dry, free-flowing powder containing from 68% to about 85% by weight of choline chloride, according to claim 7, De stap waarin deze poedervormige additief tegelijkertijd in de droogkamer wordt gevoerd met de binnenkomende luchtstroom als een aparte feed.

Referenties geciteerd patenten in de Verenigde Staten 2,765,231 10/1956 Plitt 992 2,879,161 3/1959 Vallentine 99-2 Buitenlandse patenten 1,307,421 9/1962 Frankrijk.

Andere referenties Chemische samenvattingen, 59:447 (1963). Watkins, T. C., et al., Handboek van insecticide stof 25 Verdunningen en dragers, Dorland (1955) P. 4.

Sam Rosen, Primaire onderzoeker.

s. ZANGER, Assistent -onderzoeker.