Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
tjs~7~7~
The present invention relates to calcium ammonium lact-
ate and a process for its preparation. This application is a
divisional application o~ Patent Application No. 363,866 filed
November 3, 1980. As described in that parent application calcium
ammonium lactate is a constituent formed in the preparation of
solidified forms of fermented ammoniated condensed whey. However,
the compound is a useful nutrient on its own.
BACKGROUND OF THE INVE~TION
FACW is a liquid feed supplement which is
manufactured by fermenting whey with lactic acid
producing bacteria, such a Lactobacillus bulqaricus,
ln the presence of ammonia. The fermentation of whey
converts carbohydrate to lactic acid, which is
neutralized by ammonia to form ammonium lactate. The
fermentation also multiplies the bacteria, which
consequently provide additional protein. The
fermentation product, which typically will contain 6
to 16% solid matter, is then concentrated by
evaporation typicaLly to a solids content of 40 to
6~%.
Since ruminant animals can utilize ammonium
salts as a source of n~trogen or synthesis of
protein, FACW i8 useful as a feed supplement for
them. As a liquid, it can be applied to other ration
components, such as shelled corn silage, oats, or oil
seed meals. It would be useful, however, to have F~CW
available in a solid form, for example, for use on
farms which are not equipped to use liquid feed
; supplements.
~C
,, ~
'
~ S~7~
Protein supplement and mineral blocks,
pellets or other feeds processed via binding are
normally made with expensive presses using binders
such as molasses, lignin sulfonate or bentonite.
These methods often require steam conditioning of the
meal prior to pressing and the application of high
pressure (2000 to 3000 psi). The method of the parent application
while compatible with this equipment, is a basic
improvement in that this equipment is not necessary
and little or no pressure or heat need be applied to
form blocks. This invention offers considerable
savings of time, ener~y and capital over current
practices.
SUMMARY O:F THE INVENTION
In accordance with the invention of the aforementioned
parent application FACW or other liquid substances containing
similar concentrations of ammonium lactate and total solids
can be solidified by mixing it with certain calcium
salts. Depending on the salt used and the conditions
of addition, substantial amounts of heat can be
generated. At elevated temperatures the FACW or
ammonium lactate-containing substance can be main-
tained as a liquid. The rate of solidification in
turn can be regulated by controllin9 the rate and
extent of cooling. For example, with calcium
chloride, the mixture typically begins to thicken at
~5 to 30C and can solidify completely within an
hour, The solidified product reaches maximum hardness
after one to several days. This hardening is not
associated with evaporation of water, since it w$11
occur in an air-tight package.
The method is applicable to the manufacture of
solid FACW in various forms. In its raw form,
st7t~ ~
it can be solidified in molds to form lick blocks or cubes, or it
can be extruded to produce pellets or granules. The solidified
material can be crushed to form a powder or it can be "shaved" to
produce flakes.
Trace ingredie~ts such as minerals, vitamins or drugs can
also be added to the FACW prior to processing. Substantial amounts
of molasses, corn steep liquid or other feed ingredient also may be
added.
The aforesaid composi-
tions may be used to make animal feed products in which they bind
products such as grains, roughage and forage materials into blocks,
cubes or pellets~ The compositions serve as excellent binding
agents when blended in liquid form with those products and
permitted to solidify. Typically such mixtures will contain 20 to
40% FACW and 1 to 3~ added calcium. Prior to solidification the
mixtures can be poured and/or compressed into range blocks or cubes
or extruded to form pellets. The compressed mass can then harden
in twenty minutes or less. Unlike conventional binders these
compositions are believed to serve to "cement" the solid product
particles rather than serving as a simple "adhesive". For this
reason the application of excessive pressure is not required to
achieve solidification.
Thus the method of the parent application involves pro-
ducing a ruminant animal feed which comprises solidified fermented
ammoniated condensed whey which method comprises
,, ,
~. :
~)
3a
~a) mixing fermented ammoniated condensed whey with an
effective amount of a calcium salt of a strong mineral acid to
cause the solidification of said fermented ammoniated condensed
whey, and allowing the resulting mixture to stand until it has
solidified; or
(b) mixing fermented ammoniated condensed whey with a calcium
compound which is reactive with a strong mineral acid to form a
calcium salt of said strong mineral, adding a strong mineral acid
to neutralize said compound, the amount of said calcium compound
being effective to cause solidification of said fermented ammoniated
condensed whey, and allowing the resulting mixture to stand until it
has solidified.
This invention is concerned ~ith the novel compound
calcium ammonium lactate. The method for producing the compound
comprises reacting lactic acid with ammonia in the presence of a
calcium compound.
MECHANISM OF SOLIDIFICATION
As previously described, FACW contains ammonium lactate
as a primary constituent. It can exist as a solid, but since it is
~0 highly hydroscopic it remains li~uefied under normal atmospheric
conditions. The mechanism by which FACW is solidified by the in-
vention is not fully understood. However, it is believed to
involve the formation of calcium ammonium lactate dihydrate (CAL),
a solid crystalline substance. As presently understood, solvated
calcium combines chemically with the ammonium lactate in FACW,
resulting in the production of the CAL salt which crystallizes
l~ 7 ~ ~ ,
and/or precipitates in mass to effect total solidification.
It has been found that in some cases, calcium ammonium
lactate forms as a byproduct in the manufacture of FACW. The CAL
sometimes deposits in manufacturing equipment as a sediment, for
example in pipes or storage vessels. This deposition can be pre~
vented by removing calcium from the whey used to make FACW. Such
removal can be accomplished by ion exchange, prior to fermentation.
A suitable ion exchange system is the resin Amberlite* 200.
Conversely, CAL can be obtained by purification of FACW, i.e., by
separating CAL crystals from FACW to obtain substantially pure CAL.
Calcium ammonium lactate salt (CAL) has been synthesized
in the laboratory in the following manner: 500 parts by volume of
the solution in lactic acid is neutralized with 257 parts of
aqueous ammonia (27.7% NH3) and 5.55 parts by weight of Ca(OH)2 or
(1.1 parts CaC12 2H20). The mixture i5 cooled to room temperature,
pH adju8ted to 6.8 with 1.0 NaOH solution and diluted to 1 liter
with water. After standing 4 to 7 days, well-formed crystals will
form u~ually, however, seeding with CAL crystals and agitation may
be necessary. The total crystal yield is approximately 5% by
weight of the prepared solution.
The chemical composition of the resulting salt is as
follows:
* Trade Mark
7~ ~
. .
s
Constituent Percent
Calcium B.6
Ammonia Nitrogen as N~4 7.7
Lactic Acid expressed as C3H503 74.4
Water 11.1
Total102.8
lAverage of 6 determinations.
The empirical formula of the compound based
on the above analytical data is Ca~NH4)2
(C3H503)4 2H20, Unequivocal confirmation o~ ~his
empirical formula has not been made.
The crystalline solid is characterized by
monolithic symmetry. The compound does not have a
distinct melting point, but appears to lose waters of
lS hydration at 120C and decompose at l90iSC. CAL is
very soluble in water, slightly soluble in aqueous
ammonia and insoluble in ethanol. The solid has a
specific gravity of 1.47.
Calclum ammonium lactate is useful in its own
right ac a feed supplement for ruminant animals, CAL
contains approxi~ately 37.4 percent by mass of crude
protein equivalent and the lactic acid constituent can
serve a3 a valuable source of metabolizable energy.
Calcium is an essential mineral of ~reat nutritional
importance. All of the constituents contained are
valuable sources of animal nutrition making CAL a
concentrated feed supplement that contains total ~eed
value.
DETAILED DESCRIPTION
The invention of the parent application is appli-
cable to FACW obtainable from various types of whey and
having a variety of compositions. FACW contains, as speci-
fied
i5~7'~
--6--
in section ~573.450 of the Federal Register, 35 to 55%
ammonium lactate.
The calcium salts which are used in
accordance with the invention are salts of strong
mineral acids, such as calcium chloride, calcium
sulfate and calcium phosphate. Calcium chloride is
preferred, being effective in smaller quantities, and
producing harder products, than calcium sulfate, which
in turn is more effective than calcium phosphate.
Effectiveness is believed to be correlated with water
solubility. It is possible also to use alkaline
calcium salts such as calcium carbonate, calcium oxide
or calcium hydroxide. However, when alkaline calcium
salts are used, a mineral acid must be added in an
amount sufficient to neutralize, so that the FACW is
not rendered alkaline, so as to prevent loss of
ammonia. Preferably sufficient mineral acid is added
to form the calcium salt with all of the calcium.
The amount of calcium required to solidify an
FACW-containing feed to any specified hardness
generally has to be determined experimentally. It has
been found that 6 to 10~ calcium, by weight of FACW,
i8 generally sufficient. This amount is the
percentage o calcium. The amount of any particular
calc~um salt must be adjusted to give the appropriate
amount o calcium.
The most elementary application of the method of the
parent application is the solidification of FACW. The FACW and
¢alcium salt are mixed at room temperature to dissolve
0 the 8alt and the mixture poured into a suitable mold
or hardening. It is best to slowly add this salt
while vigorously mixing FACW to eliminate clumping and
hasten its solution. If an alkaline calcium salt is
used in combination with mineral acids, as described
above, the acids are best added to the FACW during
.... ,, .. .. ,, . _ .....
l~tjst~
~;
agitation followed by the slow addition of the
alkaline salt. If calcium chloride (CaC12 2H20) is
used singly or if mineral acids are added prior to the
addition of an alkaline salt, extensive heat is
generated Calcium chloride has a positive heat of
solution and typically produces a temperature ~ise of
1 to 1.5C (2 to 3F) for each percent of the
dihydrate added. When mineral acids are used in
combination with alkaline calcium salts, the heats
generated result primarily from the solution of the
acids. The neutral~zation of the acidified FACW by
the alkaline salt is not significantly exothermic. A
rise o 1.5C (3F) is typically observed for each
percent of mineral acid (95% H2SO4 or 85% H3PO4)
added.
The FACW-calcium mixture can be maintained as
a free flowing liquid if the temperature is maintained
above the temperature at which solidiication is
spontaneously initiated. This critical temperature is
typically 25 to 30C but can vary depending on the
exact composition o the FACW, the calcium salt used,
the amount of calcium added and the rate of cooling.
If the FACW prior to calcium addition is at room
temperature (20C), the elevated temperatures obtained
following typical additions of calcium chloride or
mineral acids plus alkaline salts is sufficiently high
to maintain the FACW-calcium mixture in a liquid
state. For example, if an FACW-calcium mixture is to
contain 20% by mass o the d~hydrate, with a tempera-
ture o 20C prior to blending, the temperature of themixture will be typically 40 to 50C following com-
plete solution o the calcium salts. Such a mixture
will remain as a liquid for a prolonged period, unless
it is cooled. If the additions do not result in a
mixture having a temperature that is greater than the
6'j~7'~
critical solidification temperature, sufficient heat
must be applied to the FACW fraction before blending
to prevent premature solidification.
By regulating the rate and extent of cooling,
the rate of solidification can be controlled.
Relatively rapid solidification can result if the
fluid is cooled at a specified rate to a temperature
that nearly equals or is slightly lower (supercoolingJ
than the critical temperature before being poured into
a mold, Once the critical temperature is attained,
the product can be maintained as a liquid for a period
of approximately 2 to 5 minutes, which is sufficient
time to transfer the slightly thickened ~luid from the
mixing vessel to the solidification mold. Once
solidification is initiated, a hard, dry product can
result in about 15 minutes or less. The exact rate
and extent of cooling employed when applying this
method must be determined experimentally and will vary
with the formulation used and the FACW composition,
It is necessary to control the rate of cooling so as
to permit mold pouring at the critical temperature or
during the supercooling phase. If cooling is too
rapid, solidification can result prematurely and the
method cannot be applied to attain the desired result,
Rapid solidification is desired when
insoluble materials such as minerals or grain
fragments are slurried or suspended in liquid FACW
prior to initiating the solidification process, When
the process is controlled to produce rapid solidifica-
tion the suspended material can be homogeneously
distributed in the finished solid. This process is
especially applicable to the production of lick blocks
containing insoluble matter where the matter must be
homogeneously suspended.
7 ~ f~
If the FACW mixture to be solidified contains
no suspended solid matter, it may be desirable to
implement a slow-setting procedure. This procedure is
simpler to employ, since careful regulation of the
cooling rate is not necessary. The FACW-calcium
mixture is simply maintained at a temperature that is
greater than the solidification temperature, poured
into an appropriate mold and permitted to cool
(usually under ambient conditions) until the
solidification temperat~re is attained and
solidification is achieved. With this method,
solidification usually occurs in from 1 to 6 hours
depending on the formulation used, the initial
temperature of the fluid and the cooling conditions.
Generally the temperature at which the fluid is poured
should be at least 2 to 5C above the known
solidification temperature so as to avoid premature
solidification that could occur if pouring were
attempted at a slightly lower temperature. If the
temperature is more than 5C above the known
solldification temperature, solidiication will be
delayed.
In addition to the production of solidified
F~CW in molds, this method can be applied to the
production of FACW pellets or cubes using commonly
known extrusion type devices. To apply these device~
to liquid FACW-calcium mixtures at elevated tempera-
tures, the mixtures must be cooled to the point at
which solidification is initiated ~or supercooled) and
forced through the extrusion device precisely when the
desired consistency is attained. When using such a
process, the rate and extent of cooling have to be
carefully regulated so that the material is thickened
to a desirable consistency just prior to being forced
through the die of the extrusion device. After it has
7 f
--10--
been formed, th~ extruded material can harden completely within
minutes. The exact timing must be determined by trial for each
formulation used.
FACW solidification can be conducted also with the in-
clusion of other nutrients, such as molasses, corn steep liquid,
yeast extract products, minerals and vitamins. In
addition, drugs added to feed products may be included
depending on the final use of the product. For
example, Rumensin could be added to blocks, pellets
or cubes for feeding cattle. In general, larger
amounts of calcium salt are needed to attain a desired
hardness when the FACW contains excessive amounts of
molasses than when the process is practiced with FACW
itself. Mix~ures containing up to 25 parts by weight
of molasses for each 100 parts of FACW may be
solidified using conventional amounts of the calcium
salts. Higher levels than 25 parts of molasses may be
used, but the level of calcium may have to be
elevated. Other ingredients may also influence solid-
ification, and trial and error must be implemented to
determine the level of calcium required to effect
hardening.
A more sophisticated application of this
method i~ the use of FACW-calcium mixtures to bind
forage, roughage and other plant products when
producing protein-concentrate pellets, cubes or range-
blocks. It is best to premix the FACW and calcium
salt maintaining the temperature high enough to
prevent premature solidification, blend the resulting
mixture with the ruminant animal feeds again
maintainlng an elevated temperature, and compress the
blend in a mold or apply extrusion-type processing.
In such products it is generally desirable to include
about 30 to 40% by weight of the FACW-calcium salt
ll
mixture. The exact amounts of FACW and calcium
required for solidification will vary with the nature
of ~he ingredients included in the formulation, and
the desired hardness of the block. The exact
formulation must be determined experimentally for each
intended binding application.
When feeds of this type are produced using
FACW, the regulation of temperature during production
is critical to the success of the process. Solidifi-
cation of the FACW fraction must be prevented untilthe feed mixture is fully blended and compacted or
extruded to its final shape by maintaining it above
the solidification temperature. If solidification is
premature, the ingredients will not bind adequately.
Generally if the li~uid FACW-calcium premix
and the plant ingredients are blended rapidly and
compressed or processed immediately, a well bound
product will result, even without auxiliary heating.
Generally, when the liquid FACW-calcium mixture is at
40-50C, and it i8 blended in normal proportions with
the plant product mixture at room temperature, the
temperature of the resulting blend is low enough to
initiate solidification of the FACW-calcium fraction,
However, the mixture generally will remain suffici-
ently moist and sticky to permit good compaction tooccur or a period of approximately 5 to 10 minutes.
If the blended feed is to remain for an extended
period of time before compression processing, the
total feed must be heated so as to maintain it above
the solid~ication temperature.
After blending the FACW, calcium salt and
plant ingredients, the mixture is compressed in the
desired form and left to harden by the solidification
of the FACW. During ~ormation sufficient pressing
must be applied to compact the product to a convenient
. ~
.
7'~
-12-
density, i.e., remove extraneous pockets of air. If
the solidified product is not to cure or be stored in
a mold, sufficient pressure must be applied to
maintain the shape of the product until solidification
is sufficiently complete to allow the shape to be
maintained before the product is removed from the
mold.
The following examples illustrate the method wherein
calcium ammonium lactate was used in the preparation of solid whey.
All parts and percentages are given on a weight basis, unless
stated otherwise.
EXAMPLE _
The following formulation was used to produce
a 30-pound lick-type range block:
Inqredient Percent
FACW (60% solids) 80
CaC12 2H20 20
100
A 5-gallon bucket was used as a mixing
vessel, with agitation from an air-driven barrel mixer
fitted with a single set of three 2-inch blades. The
mixlng vessel was placed within a 15-gallon tub which
was filled with water for rapid cooling of the blended
feed ingredients. The mold used to shape the lick
block was a 3-gallon plastic tub (6 x 11 x 14
inches). Utilization of the plastic tub permitted
easy removal of the finished block, since the inside
walls were smooth and slightly tapered at the open
end.
The CaC12 2H20 fraction (6 pounds) was
poured slowly into the vigorously mixing FACW fraction
~24 pounds), The mixture was agitated for approxi-
mately 5 minutes to assure complete solution of the
added salt. After mixing, the temperature of the FACW
mixture was elevated 33C from room temperature to
13
approximately 56C. After the initial 5 minutes of
mixing, cold tap water was circulated through the
cooling vessel and the fluid cooled at an approximate
rate of 1.5 i 0.5C per minute. The fluid mixture
began to thicken when a temperature of approximately
31C was reached, and it was immediately poured into
the mold for solidification. The mixture hardened in
about 10 minutes and was removed from the mold after 1
hour. The block attained maximum hardness after two
or three days of curing.
The finished block was chemically analyzed
and observed to contain the following:
Constituent Percent ~/M)
CPE 36.3
CPE from non-protein nitroaen 31.6
Lactic acid 29.8
Estimated solids 68.0
Calcium 5.85
This block was fed free-choice to a herd of
heifers and dry cows under normal field conditions and
was observed to provide adequate palatability and
weatherability.
EXAMPLE II
A 30-pound lick-type block similar to that of
Example I was prepared with the inclusion of black
strap molasses from the following formulation:
Ingredient Percent
FACW (60~ solids) 70
CaC12 2H2O 20
Molasses, Black Strap ~ 10
100
The procedure used to produce this block was
similar to that employed in Example I. The FACW and
r--~7r~r~J
14
molasses were premixed, then the calcium salt was
added as previously described. This material required
approximately six hours to solidify and several days
to attain maximum hardness.
The finished block was chemically analyzed
and observed to contain the following:
Constituent Percent
CPE
CPE from non-protein nitrogen 28.4
Lactic acid 27.9
Estimated solids 69.5
Calcium S.78
This block when used in the field as a lick-
feed was palatable and weathered well.
EXAMPLE III
The following formulation was used to produce
a 30-pound FACW range block using calcium carbonate
plus acids for solidification:
In~redients Percent
FACW (60% solids) 68
CaCO3 15
85% H3PO4 15
95% H2S~4 2
100
In addition to neutralizing the alkaline
effect of the carbonate, the acids served as a
valuable source of phosphorus and sulfur.
This block was prepared using the apparatus
described in Example I. The acids were first added to
the FACW and mixed. Following the addition of the
acid, the temperature of the mixture rose from 23C to
48C. The CaCO3 was next added slowly to the warm
FACW-acid mixture over a period of about 15 to 20
minutes. Extensive foaming, resulting from the
production of carbon dioxide, was observed during and
7'~
following the addition of CaCo3. Slow addition was
used to control the neutralization reaction and
prevent excessive foaming. After carbonate addition
was completed, the blend ~ontinued to produce gas
slowly for periods exceeding one hour.
After one hour, cooling was initiated. The
liquid began to thicken when a temperature ~f about
27C was attained, and it was immediately poured into
the mold.
Carbon dioxide production continued after the
thickened liquid was transferred to the molds, and the
solidifying product expanded as the evolved gases were
entrapped. The volume of the dried block was about
50~ larger than the freshly poured product. The
product solidified in about six hours and attained
maximum hardness afte~ several days of curing.
The finished block was chemically analyzed
and found to contain the following:
Constituent Percent
CPE 31.9
CPB from non-protein nitrogen 27.5
Lactic acid 26.2
Estimated solids 70.5
p~ 5.70
Calcium 6.42
Phosphorus 4.85
Sulfur 0.52
EXAMPLE IV
A 30-pound range block similar to that
described in Example III was produced, with the
inclusion of low moisture shelled corn, using the
following formula:
., .u, ~
i~ 3 7 f ~
16
Ingredient Percent
FACW (60% solids) 52.2
CaCO3 12.0
85~ H3PO~ 12.0
95% H2SO4 1.6
Ground corn, LMS 20.0
100
The procedure implemented was similar to that
described in Example III. The corn fraction was added
to the other premixed ingredients just prior to
initiating the cooling operation. A temperature rise
of 22C was observed during preparation of the
premix. Solidification was initiated after cooling to
approximately 32C. The thickening product was not
poured until it had attained a consistency that would
permit suspension of the corn fragments. The
solidification was completed after about 6 hours and
maximum hardness was attained after several days of
curing. The block matter was physically similar to
that produced in Example III, and the corn particles
appeared to be uniformly distributed within the
product,
The finished product was observed to contain
the following:
Constituent Percent
CPE 28.5
CPE from non-protein nitrogen 22.6
Lactic acid 22.3
Estimated solids 74.0
pH 5.51
Calcium 4.50
Phosphorus 4.43
Sulfur 0.26
~ ~ ~; 5 7 ~ ~
17
EXAMPLE V
A 200-gram high soy range cube was produced
with FACW plus calcium serving as the binding agent
using the following formulation:
Ingredient Percent
Soybean meal 65.7
FACW (60% solids) 28.1
CaC12 2H2O 6.2
100
The FACW and CaC12 ingredients were premixed
with vigorous mechanical agitation for about 5
minutes. This premix was then blended with the
soybean meal in a 500-liter stainless steel beaker
using a large metal spatula. Blending was conducted
for 3 to 5 minutes (just long enough to attain mixture
uniformity) and immediately transferred to a 400-ml
plastic beaker which served as a solidification
mold. The blend was tightly packed by hand pressure,
covered with plastic film and permitted to remain
undisturbed for several hours before removing the
mold. The mixing and packing operation employed in
this example was sufficiently rapid to avoid premature
solidification. The product was sufficiently moist
and sticky at the time of packing to attain good5 binding.
The finished product was dry, observed to be
of a desired hardness, and displayed good weathering
characteristics. The finished product was estimated
to contain the following:
Const_tuent Percent
CPE 42.5
CPE from non-protein nitrogen 9,9
Lactic acid 10.1
Estimated solids 80.1
Calcium 1.90
tj~t~7
18
EXAMPLE VI
A 200-gram soy range cube similar to that
described in Example V was prepared with the inclusion
of black strap molasses, usinq the following formula:
Ingredient Percent
Soybean Meal 59.1
FACW (60% solids) 25,3
Molasses, Black Strap 10.0
CaC12 2H2O _ 5.6
100
The preparation of this cube was similar to
that produced in Example V. The molasses was premixed
with the FACW prior to the addition of the calcium
salts. This product was also dry, observed to display
desired hardness and had good weathering
characteristics. The finished product was to contain
the following:
Constituent Percent
CPE 3B.5
CPE from non-protein nitrogen 8.91
Lactic acid 9.11
Estimated solids 81~8
Calcium 1.80
EXAMPLE VII
Range blocks similar in composition to
commercially produced protein blocks were produced
using F~CW and CaC12 as binding agents in the
following three formulations;
. , , . . ,, , .. , .,, .. , ... .~, . ... . .
19
Percent
IN~REDIENTS B~XX 1 B~X~ 2 B~X~ 3
Soybean o~ meal 47.9 40.4 39.3
FACW 26.7 32.8 ~.1
Dehydrated alfalfa 9.209.20 9.20
Linseed meal 1.83 1.83 1.83
Calcium ~oride, dihydrate 5.857.20 9.00
Amm~nium p~yphosphate 3.113.11 3.11
Amnonium sulfate 0.5480.548 0.548
Sodium chloride 4.57 4-57 4-~7
Zin~ sulfate, heptahydrate 0.124 0.124 0.124
M~anese sulfate, m~nohydrate .0496 .0496 .0496
Ferric sulfate .0578 .0578 .0578
~agnesium sulfate, dihydrate 0.122 0.122 0.122
15 Cupric s~fate .0952.09S2 ,0952
Cobalt sulfate .00194.00194 .00194
Scdium iodide .00066.00066 ,00066
Vitam~ns ~ #
~arAI, 100 100 400
20 #50,000 and 12,500 U.S.P. units of Vitamin A and
Vitamin D3, respectively, added per pound of block.
The FACW and CaC12 components were premixed
and added collectively to the remaining dry
ingredients, which were also premixed. The FACW-CaC12
25 premixes were prepared in a 2-gallon plastic bucket.
Each FACW fraction was blended vigorously with a
Grohav air mixer fitted with a single set of 2-inch
blades during the slow addition of each respective
CaC12 fraction. Rapid mix~ng and slow addition was
30 used to prevent agglomeration and clumping of the
CaC12. Each FACW-calcium premix was mixed for about
five minutes after the addition to assure that CaC12
had been totally dissolved. The temperature of each
FACW fraction was elevated during the premixing
i5'~
operations in which CaC12 was added. The temperature
of the premixes were elevated about 20C with the 22%
additions of CaC12 2H20.
The premixing of the dry ingredients was
conducted in a Davis batch horizontal ribbon-type
mixer (Model ~S-l) with a mixing capacity of five
cubic feet. The liquid premix was poured slowly and
uniformly onto the mixing dry ingredients to help
assure uniformity of mix. After the liquid addition
was completed, the mixing was continued for an
additional five minutes. Any feed that was sticking
in excess to the ribbon blades or remaining stagnant
in the lower corners of the mixer was then removed
with a metal spatula and mixing was continued for an
add$tional five minutes.
Each of the blendings of feed ingredients
mixed loosely and freely in the horizontal ribbon
mixer. The mixtures prepared to produce blocks 1 and
2 (27 and 33% FACW, respectively) were moist and
slightly sticky. The block 3 mixture (41% FACW) was
noticeably more moist and sticky. Before solidifica-
tion, the block 3 mixture was wet and almost paste-
like. Even though the three mixtures blended
uniformly without clumping, they were observed to pack
tightly if compressed in one's hand.
Excessive mixing times had to be avoided,
since solidification of the feed mixes initiated in
about 15 minutes or less. If not removed from the
mixer expeditiously, the mixtures were observed to
form a hard, relatively dry crust on the back side of
the ribbon blades and on the mixer walls in areas of
stagnant mixing. Also, if mixed excessively, the feed
mixtures were observed to dry to an extent that did
not permit adequate packing, i.e., the feed particles
lost their adhesive nature.
g ~ "~J
21
The moist, freshly-prepared feed ~lend~ were
easily packed with good uniformity into the block
mold. Some disuniformity was observed in the density
of the pack due to the layered addition of the feed
mixture, i.e., the top portion of each strata was
observed to be slightly more dense than the bottom
portion. The moist feed materials prepared ~o produce
blocks 1 and 2 compressed to very firm solid masses
that were not easily crumbled. The block 3 mix~ure
remained somewhat soft and pasty immedi~tely after
packing.
The feed mixtures were removed immediately
from the mixer and packed into a block solidification
mold. The mold was a rectangular wooden box,
constructed to approximate the shape and size of most
commercial range blocks. The faces of the mold were
held together by screws so as to permit the disas-
semblement of the box for easy removal of the finished
block. The open end from which the mold was filled
was filled with a movable lid that fit within the
box. After f~lling, a 25-pound weight was placed on
the movable lid so as to apply a constant pressure to
the solidifying feed mixture.
Each feed mixture was packed manually in the
golidification mold with the butt end of a 4-foot
length of 4 x 4" board weighing approximately ten
pounds. The wet feed was added to the box in
fractions weighing 1-2 pounds each with each fraction
being thoroughly tamped ~packed) before the addition
of each subæequent fraction. Once the mold was filled,
the lid was placed on the exposed feed surface and
weighed.
Even though the feed blends were left in the
mold ~or 4 to 6 hours, it appears that blocks 1 and 2
would retain their shape and remain firm if the mold
was removed immediately after packing. The blocks
22
would likely maintain some surface stickiness but
would probably be resistan~ to crumbling and
breakage. After being compressed into the form of a
block, they could be immediately packaged and stacked
without being damaged.
~ he mold was removed from block 1 with little
difficulty. The mold was easily freed from the block
mass with little resistance and little feed remained
adhered to the wood. The block surface was dry and
10 firm. The mold, however, was not easily removed from
blocks 2 and 3. Considerable force was needed to pull
away from the wooden mold from block 2. Large
fragments of the hardened feed adhered to the wood and
were torn from the block. The block surface was still
15 sticky but remained firm. This problem possibly could
have been alleviated if the mold were lined with sheet
plastic or other non-stick surface prior to filling.
Block 3 adhered even more firmly to the wood mold. A
metal spatula had to be forced between the block and
the mold to release it. The block surface remained
very sticky and although it was firm, an impression
could be made in it with the force of a person's
thumb,
After being bagged and allowed to stand for a
25 one-week curing period, all of the blocks were very
hard and dry and displayed no surface stickiness The
blocks as a whole were not easily crumbled, but some
crumbling was observed at the edges of the block
surfaces.
Chemical analysis of the blocks provided the
following information:
~i! ;. i~f~iS7
23
NUTRIENT Block 1 Block 2 Block 3
Crude protein equivalent 39.5 38.1 36.3
CPE derived from NPN 12.4 15.4 17.7
~ Lactic acid 10.5 12.8 17.6
5 % Drymatter 83.8 81.7 78.3
p~ 5.68 5.64 5.57
% Ash 12.1 12.8 15.4
% Calcium 1. 64 2.13 2.37
% Phosphorus O . 91 0 . 69 0 . 71
10 % Sulfur 0-07 0.10 0.18
~ Sodium 1.58 1.41 1~98
% Chlor ide 7 . 8 10 11
The blocks were fed and consumed by cattle in
approximately the correct amount for their size and
15 basal ration. These blocks weathered well and were
judged to be equivalent to normal feed blocks.
This process is not restricted to these
examples or devices but could be carried out using
commercially available food and feed industry
20 equipment by control of temperatures, FACW level and
calcium level. ~he molds used could be any
commercially available contai~er provlded it was
sufficiently rigid. Pressing of the materlal into the
mold could be by any device such as cheese block
25 presses or other such commonly used device. Feed
block presses could also be used but high pressure is
not required.
