Food or edible material: processes – compositions – and products – Products per se – or processes of preparing or treating... – Protein – amino acid – or yeast containing
Reexamination Certificate
1999-06-03
2001-01-23
Sayala, Chhaya D. (Department: 1761)
Food or edible material: processes, compositions, and products
Products per se, or processes of preparing or treating...
Protein, amino acid, or yeast containing
C426S471000, C426S654000, C426S805000, C426S807000
Reexamination Certificate
active
06177124
ABSTRACT:
The present invention relates to an active-substance concentrate, the process for its preparation and its use.
It is known to prepare mixtures consisting of choline chloride and precipitated silica by mixing an aqueous solution of choline chloride together with at least 2% hydrophilic silica and at least about 3% water-repellent silica, whereby, however, the mixing process is concluded so long as silica still rises to the surface of the mixture after an interruption of the mixing movement, and by subsequently spray-drying this mixture (DE-A 22 09 477).
The known mixture consisting of precipitated silica and aqueous choline chloride solution has the disadvantage that a sufficient stability in storage is not ensured without impairing the flowability.
It is furthermore known to prepare powders containing choline chloride by atomizing an aqueous choline chloride solution in a spray tower, in which connection a cloud of finely divided hydrophobic precipitated silica (SIPERNAT D17 produced by Degussa AG) is present in the spray tower. In the process the hydrophobic precipitated silica is deposited on the surface of the choline chloride particles. The product obtained is dried in a fluidized-bed drier. It has an active-substance content amounting to 95.8 wt.-% (DE-A 42 18 768).
The known powder that contains choline chloride has the disadvantage that it is stable in storage only for a few days. Water is secreted from the product after as little as 24 hours.
It is therefore an object of the invention to prepare a mixture consisting of silicon-dioxide variants and active-substance solution, in particular aqueous choline chloride solution, that is stable in storage over a relatively long period and remains flowable.
SUMMARY OF THE INVENTION
The above and other objects of the present invention can be achieved in the form of an active substance concentrate that has the following characteristics:
a) active substance content: 85 to 98 wt.-%, preferably 93 to 97 wt.-%
b) hydrophobic silica/silicate 2 to 15 wt.-%,
c) water (upon discharge maximally 0.5 wt.-% from the drier):
d) stability in storage: at least 1.5 years with an equilibrium water content
e) free-flowing powder.
By way of silicon dioxide variant, precipitated silicas, pyrogenically prepared silicas and/or silicates may be employed. All of these products are known in the art.
These substances are known from Ullmann's Enzyklopadie der technischen Chemie, Volume 21, 4th Edition, pages 462 to 476 (1982).
In a preferred embodiment of the invention the active-substance concentrate may contain choline chloride by way of active substance.
Further active substances may be hygroscopic substances from the food sector, such as hydrolyzed vegetable protein for example, hygroscopic substances from the animal-feedstuff sector, such as iron sulfate for example.
A further aspect of the present invention resides in a process for preparation of the active-substance concentrate, comprising forming a master-batch suspension with a content of 10 to 15 wt.-% of hydrophobic silicon-dioxide variant, in particular with the hydrophobic precipitated silica Sipernat D10, and 85 to 90 wt.-% of a 40 to 80-% aqueous active-substance solution, in particular 70 to 80-% aqueous choline chloride solution. The master batch is firstly produced by mixing the constituents in the form of a reversal emulsion, for example with the aid of a dissolver disc which keeps the suspension in motion, and/or intensive mixing with the aid of a bead mill with cooling device (Dyno mill). This master-batch suspension formed thereby is optionally diluted with water or with further aqueous active-substance solution and is subsequently spray dried by means of any suitable equipment therefor.
A mixing device that subjects the material to be blended to a forced supply and generates a high shear effect can be employed with particular advantage.
DETAILED DESCRIPTION OF INVENTION
Further details of the present invention are presented below. In carrying out the invention a variety of silicas can be used.
By way of example, hydrophobic precipitated silicas, precipitated silicas that are made water-repellent by known processes may be employed.
The water-repellent precipitated silica, known by the trademark SIPERNAT D10, may preferably be employed. This precipitated silica is characterised by the following physicochemical characteristic data:
SIPERNAT D10
(hydrophobic)
appearance
loose white powder
surface area according to BET
1)
m
2
/g
90
mean particle size
&mgr;m
5
compacted bulk density
2)
g/l
100
drying loss
3)
(2 h at 105° C.)
%
3
ignition loss
4)8)
(2 h at 1,000° C.)
%
7
9)
pH value
5)
(in 5-% dispersion)
10.3
10)
SiO
2
7)
%
98
Na
2
O
7)
%
1.0
SO
3
%
0.8
C
7)
%
3.0
methanol wettability
%
about 60
oversize material
6)
(acc. to Mocker, 45 &mgr;m)
%
0.01
1)
acc. to ISO 5794/1
2)
acc. to DIN ISO 787/11, JIS K 5101/21 not sieved
3)
acc. to DIN ISO 787/2, ASTM D 280, JIS K 5101/21
4)
acc. to ISO 3262/11, ASTM D 1208, JIS K 5101/23
5)
acc. to DIN ISO 787/9, ASTM D 1208, JIS K 5101/24
6)
acc. to DIN ISO 787/18, JIS K 5101/20
7)
relative to the substance ignited for 2 hours at 1,000° C.
8)
relative to the substance dried for 2 hours at 105° C.
9)
includes about 3% chemically bonded carbon
10)
in water: methanol 1:1
Instead of the hydrophobic precipitated silica, hydrophobic, pyrogenically prepared silicas or hydrophobic silicates may also be employed.
Mixing of the constituents with a view to producing the master-batch suspension is effected with shear forces that permit a phase reversal—that is to say, a rewetting of the surface of the precipitated silica—to be achieved. This phase reversal signifies a complete wetting of the hydrophobic precipitated silica with the aqueous active-substance solution without addition of wetting agents.
Premixing may preferably be carried out by means of a dissolver disc; the definitive preparation of a premix may be carried out, in particular, by means of a bead mill. Drying is preferably effected by spray drying.
The active-substance concentrate according to the invention presents the following advantages:
In the course of storage no change occurs in the physical properties such as stability in storage, grain size or flowability, despite a maximum increase in weight amounting to 33% moisture from the air. The maximum absorption of water in this case is dependent on the atmospheric humidity. In this connection it is a question of an equilibrium content.
The active-substance concentrate according to the invention may be used for the preparation of premixes and mixed feeds, in which connection it serves as a feed supplement for livestock.
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patent: 4859709 (1989-08-01), Rawlins
patent: 4950488 (1990-08-01), Schweitzer et al.
patent: 5248702 (1993-09-01), Neumann et al.
patent: 5300250 (1994-04-01), Morgan et al.
patent: 5468720 (1995-11-01), Lisa et al.
patent: 5486363 (1996-01-01), Kiefer et al.
patent: 5766668 (1998-06-01), Brommedsiek et al.
patent: 1812351 (1970-08-01), None
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patent: 0253212 (1988-01-01), None
patent: 9629886 (1996-10-01), None
patent: 9632949 (1996-10-01), None
patent: 9907237 (1999-02-01), None
Grinschgl Brigitte
Oelm{umlaut over (u)}ller Rolf
Beveridge, DeGrandi, Weilacher & Young
Degussa H{umlaut over (u)}ls Aktiengesellschaft
Sayala Chhaya D.
Smith , Gambrell & Russell, LLP
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