Production and use of formulations consisting of cellulose,...

Details Production and use of formulations consisting of cellulose,... Production and use of formulations consisting of cellulose,...

1999-06-14

2001-05-15

Woodward, Ana (Department: 1711)

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

Processes of preparing a desired or intentional composition...

C426S330300, C426S330400, C426S330500, C426S422000, C426S487000, C426S592000

Reexamination Certificate

active

06232373

ABSTRACT:

The present invention relates to formulations consisting of cellulose, alkali metal caseinate and crosslinked homopolymers or copolymers of N-vinyllactams and/or polymers based on a basic N-vinyl heterocycle having a PK
a
of at least 3.8, their preparation and use for treating biological liquids of plant origin in an unfermented, partially fermented or completely fermented state.
In the production of liquid products from unfermented, partially fermented or completely fermented precursors, their stability with regard to color, aroma and taste is an outstanding feature. These three features are dependent in biological liquids of plant origin on the concentration of phenolic constituents and the content of heavy metal ions. Controlled adjustment of the concentration of these constituents is thus a critical precondition for the production of end products with stable sensory properties.
To influence phenolic substances, products have previously been used which react by complexing, adsorption or precipitation. Suitable products are native proteins such as gelatine, caseinate, egg white, ovalbumin, isinglass or dried blood, as well as modified proteins such as potassium caseinate. In addition, crosslinked polymers based on vinylpyrrolidone (Crospovidone, PVPP) are used. Thus, EP-A-088 964 describes a process for preparing insoluble polymers which are only slightly swellable in water of a basic N-vinylheterocycle and its copolymers with up to 30% by weight of copolymerizable monomer. Complexing transition metal cations to prepare catalysts based on the described polymers is proposed. These polymers have a broad spectrum of applications, especially as adsorber resins. They adsorb proteins, especially enzymes, very well, and are likewise suitable for removing interfering polyphenols and colorants from aqueous solutions by adsorption.
The native and modified proteins, as well as the crosslinked polymers, have the disadvantage that they require a certain pretreatment by swelling. This is highly time-consuming. Since the great majority of the products are removed from the medium used, together with the suspended turbidities, by sedimentation, this step is also highly time-consuming and can take up to 6 weeks. Furthermore, these products have the disadvantage that they do not remove all phenolic substances or classes of substances to the same extent, but there is in each case a preferred interaction with a certain group of phenolic substances. The sediments produced are generally slimy pasty compositions from which liquid is taken off by a downstream treatment, in order to bring them into a reutilizable or landfillable state.
It is an object of the present invention, therefore, to find a product which does not have the abovementioned disadvantages and is able to decrease the content of various groups of phenolic compounds and simultaneously also decrease the concentration of dissolved heavy metals. At the same time, the handleability should be improved by avoiding the complex preparation phase of the starting material.
We have found that this object is achieved by solid preparations consisting of
(a) from 10 to 90% by weight of cellulose,
(b) from 5 to 60% by weight of an alkali metal caseinate and
(c) from 5 to 85% by weight of a polymer selected from the group consisting of:
c
1
) an N-vinyllactam polymer obtained by copolymerization of from 90 to 99.5% by weight of one or more N-vinyllactams and from 0.5 to 10% by weight of a crosslinker or
c
2
) of a polymer of from 50 to 99.5% by weight of at least one basic vinylheterocycle having a pK
a
of at least 3.8 and from 0 to 49.5% by weight of another copolymerizable monomer as well as from 0.5 to 10% by weight of a crosslinker,
or mixtures of the polymers c
1
) and d
2
);
the invention also relates to their preparation and use.
For the purposes of the invention, cellulose (a) is the various forms of cellulose such as cellulose fibers, micronized cellulose, fibrillated cellulose or microcrystalline cellulose which have bulk densities from 0.15 to 0.45 g/cm
3
, mean fiber lengths from 15 &mgr;m to 900 &mgr;m and a mean fiber diameter from 5 &mgr;m to 50 &mgr;m.
For the purposes of the invention, an alkali metal caseinate (b) is especially potassium caseinate, which is obtained by treating casein with potassium hydroxide solution or solutions of alkaline potassium salts of organic or inorganic acids, such as phosphoric acid or citric acid.
Casein originates from short-time heat-treated skimmed milk which has a maximum fat content of 0.05%. The skimmed milk, to separate off the whey, is coagulated with acids by setting the pH to the isoelectric point of casein, 4.5±0.2. After heat treatment, separating off the whey and washing with warm water, the crude casein is obtained. This is further processed as wet curd, or after drying, to give caseinate, by solubilizing it by adding potassium hydroxide or other alkali metal hydroxides. It is dried by spray-drying or an extrusion process. The products obtained which are particularly suitable for preparing the formulations according to the invention have a water content from 5 to 10% and a protein content from 87% to 92%, as well as an ash content from 3% to 8%.
For the purposes of the invention, N-vinyllactams c
1
) are 3-methyl-N-vinylpyrrolidone, in particular N-vinylcaprolactam and N-vinylpyrrolidone (VP), which are used alone or in a mixture with one another.
The monomers c
1
) are used in an amount of from 90% to 99.5%, preferably from 98% to 99% by weight, based on the total polymer.
Suitable crosslinkers are those which contain, per molecule, two or more vinyl groups which can be copolymerized by a free radical mechanism. Those which are particularly suitable are alkylenebisacrylamides, such as methylenebisacrylamide and N,N′-bisacryloylethylenediamine, in addition N,N′-divinylethyleneurea, N,N′-divinylpropyleneurea, ethylidene-bis-3-(N-vinylpyrrolidone) and N,N′-divinyldiimidazolyl-(2,2′)-1,4-butane and 1,1′-bis(3,3′-vinylbenzimidazolid-2-one)-1,4-butane. Other useful crosslinkers are, for example, alkylene glycol di(meth)acrylates, such as ethylene glycol di(meth)acrylate and tetramethylene glycol di(meth)acrylate, aromatic divinyl compounds, such as divinylbenzene and divinyltoluene, and alkyl acrylate, divinyldioxane, pentaerythritol triallyl ethers and their mixtures. When polymerization is carried out in the presence of water, obviously they are only suitable if they are soluble in the aqueous monomer mixture.
The crosslinkers are used in an amount of 0.5-10, preferably 1-2, % by weight, based on all monomers of the polymer.
For the purposes of the invention, basic vinyl heterocycles c
2
) are saturated and aromatically unsaturated heterocycles having a vinyl and at least one basic tertiary ring nitrogen having a pK
a
of at least 3.8. In addition to the vinyl, the ring may also bear alkyls having 1 to 4 carbons, phenyls or benzyls, or else a fused second ring. Specific examples are: N-vinylimidazole (Vl) and derivatives thereof, such as 2-methyl-1-vinylimidazole, 4-methyl-1-vinylimidazole, 5-methyl-1-vinylimidazole, 2-ethyl-1-vinylimidazole, 2-propyl-1-vinylimidazole, 2-isopropyl-1-vinylimidazole, 2-phenyl-1-vinylimidazole and 1-vinyl-4,5-benzimidazole. In addition, the following may be used, for example: 2-vinylpyridine, 4-vinylpyridine and 2-methyl-5-vinylpyridine. Obviously, mixtures of basic vinyl heterocycles with one another can also be used.
Preferred monomers for this are N-vinylimidazole and 2-methyl-N-vinylimidazole.
These monomers are used in an amount of 50-99.5, preferably 60-96, % by weight, based on the total polymer.
The comonomers are copolymerized in amounts of up to 49.5, preferably up to 30, % by weight, particularly preferably up to 20% by weight, based on the total monomer mixture. Suitable comonomers are, for example, styrene, acrylic esters, vinyl esters, acrylamides and N-vinyldihydropyridines. Preferably, N-vinyllactams, such as 3-methyl-N-vinylpyrrolidone, in particular N-vinylcaprolactam and N-vinylpyrrolidone (

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